Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_section_title              
;
Versatile supramolecular self-assembly. Part I.
Network formation and magnetic behaviour of the alkaline salts of the
bis(malonate)cuprate(II) malonate anion
;

_publ_contact_author_name        'Catalina Ruiz-Perez'
_publ_contact_author_address     
;
Laboratorio de Rayos X y Materiales Moleculares
Dpto. Fisica Fundamental II. Facultad de Fisica
Universidad de La Laguna
E-38204. La Laguna. Tenerife
Spain
;
_publ_contact_author_email       caruiz@ull.es
loop_
_publ_author_name
'Catalina Ruiz-Perez'
'Fernando S. Delgado'
'Miguel Julve'
'F. Lloret'
'Joaquin Sanchiz'

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 256111'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H10 Cu Li2 O11'
_chemical_formula_weight         335.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8515(3)
_cell_length_b                   8.8520(6)
_cell_length_c                   10.5293(7)
_cell_angle_alpha                80.655(6)
_cell_angle_beta                 75.043(4)
_cell_angle_gamma                70.363(4)
_cell_volume                     579.07(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             338
_exptl_absorpt_coefficient_mu    1.940
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   '(SADABS, Sheldrick, 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  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5358
_diffrn_reflns_av_R_equivalents  0.0139
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         6.43
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2591
_reflns_number_gt                2393
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.0220P)^2^+0.2450P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2591
_refine_ls_number_parameters     221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0517
_refine_ls_wR_factor_gt          0.0501
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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 0.20931(3) 0.17940(2) 0.477458(16) 0.01831(7) Uani 1 1 d . . .
C1 C 0.2837(2) 0.21769(17) 0.72562(14) 0.0200(3) Uani 1 1 d . . .
C2 C 0.1899(3) 0.08294(18) 0.78235(15) 0.0216(3) Uani 1 1 d . . .
C3 C 0.2555(2) -0.05626(17) 0.69761(14) 0.0183(3) Uani 1 1 d . . .
O1 O 0.27566(19) 0.27556(13) 0.60746(10) 0.0229(2) Uani 1 1 d . . .
O2 O 0.26469(19) -0.03021(13) 0.57420(10) 0.0235(2) Uani 1 1 d . . .
O3 O 0.3605(2) 0.27152(14) 0.79650(11) 0.0295(3) Uani 1 1 d . . .
O4 O 0.2946(2) -0.19343(13) 0.75440(11) 0.0320(3) Uani 1 1 d . . .
C11 C 0.2527(2) 0.14563(18) 0.20377(14) 0.0187(3) Uani 1 1 d . . .
C12 C 0.1411(3) 0.32430(19) 0.18337(16) 0.0240(3) Uani 1 1 d . . .
C13 C 0.1733(2) 0.43519(18) 0.26552(14) 0.0188(3) Uani 1 1 d . . .
O11 O 0.25145(19) 0.07657(13) 0.31940(10) 0.0249(2) Uani 1 1 d . . .
O12 O 0.1739(2) 0.39162(13) 0.38749(10) 0.0259(2) Uani 1 1 d . . .
O13 O 0.33736(19) 0.07013(13) 0.10341(10) 0.0254(2) Uani 1 1 d . . .
O14 O 0.1884(2) 0.56755(14) 0.21579(11) 0.0310(3) Uani 1 1 d . . .
O1W O -0.1621(2) 0.25946(19) 0.56524(18) 0.0347(3) Uani 1 1 d . . .
O2W O 0.4152(2) 0.53939(17) 0.63269(12) 0.0250(2) Uani 1 1 d . . .
O3W O 0.6381(3) 0.2672(2) 0.99356(15) 0.0454(4) Uani 1 1 d . . .
Li1 Li 0.2942(5) 0.4979(4) 0.4962(3) 0.0311(6) Uani 1 1 d . . .
Li2 Li 0.4976(5) 0.1524(3) 0.9350(3) 0.0261(6) Uani 1 1 d . . .
H1 H 0.215(3) 0.045(2) 0.864(2) 0.026(5) Uiso 1 1 d . . .
H2 H 0.046(3) 0.129(2) 0.7916(19) 0.030(5) Uiso 1 1 d . . .
H11 H 0.177(3) 0.360(3) 0.096(2) 0.040(6) Uiso 1 1 d . . .
H12 H -0.009(4) 0.337(3) 0.208(2) 0.040(6) Uiso 1 1 d . . .
H1W1 H -0.209(5) 0.205(4) 0.561(3) 0.055(10) Uiso 1 1 d . . .
H2W1 H -0.183(5) 0.273(4) 0.637(3) 0.066(10) Uiso 1 1 d . . .
H1W2 H 0.413(4) 0.476(3) 0.686(2) 0.039(7) Uiso 1 1 d . . .
H2W2 H 0.381(3) 0.618(3) 0.667(2) 0.033(6) Uiso 1 1 d . . .
H1W3 H 0.688(4) 0.325(3) 0.949(3) 0.048(7) Uiso 1 1 d . . .
H2W3 H 0.673(4) 0.251(3) 1.060(3) 0.045(7) Uiso 1 1 d . . .

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 0.03159(11) 0.01315(10) 0.01227(10) 0.00034(6) -0.00560(7) -0.00963(7)
C1 0.0301(8) 0.0125(7) 0.0178(7) -0.0006(5) -0.0078(6) -0.0055(6)
C2 0.0339(9) 0.0149(7) 0.0154(7) -0.0002(5) -0.0033(6) -0.0089(6)
C3 0.0231(7) 0.0149(7) 0.0184(7) -0.0003(5) -0.0050(5) -0.0079(5)
O1 0.0407(6) 0.0178(5) 0.0165(5) 0.0027(4) -0.0115(4) -0.0149(5)
O2 0.0402(6) 0.0151(5) 0.0164(5) -0.0002(4) -0.0073(4) -0.0099(5)
O3 0.0546(8) 0.0209(6) 0.0230(6) 0.0037(4) -0.0211(5) -0.0174(5)
O4 0.0624(8) 0.0135(5) 0.0217(6) 0.0027(4) -0.0147(5) -0.0116(5)
C11 0.0224(7) 0.0200(7) 0.0164(7) -0.0022(5) -0.0038(5) -0.0099(6)
C12 0.0318(9) 0.0215(8) 0.0185(8) -0.0011(6) -0.0095(6) -0.0053(6)
C13 0.0206(7) 0.0168(7) 0.0158(7) 0.0005(5) -0.0021(5) -0.0038(5)
O11 0.0438(7) 0.0179(5) 0.0138(5) -0.0010(4) -0.0057(4) -0.0113(5)
O12 0.0482(7) 0.0173(5) 0.0160(5) 0.0017(4) -0.0094(5) -0.0146(5)
O13 0.0381(6) 0.0224(6) 0.0142(5) -0.0046(4) -0.0019(4) -0.0088(5)
O14 0.0510(7) 0.0196(6) 0.0207(6) 0.0042(4) -0.0047(5) -0.0139(5)
O1W 0.0290(7) 0.0276(7) 0.0429(9) 0.0002(6) -0.0036(6) -0.0076(6)
O2W 0.0389(7) 0.0164(6) 0.0215(6) -0.0036(5) -0.0056(5) -0.0106(5)
O3W 0.0791(11) 0.0558(10) 0.0235(7) 0.0138(6) -0.0195(7) -0.0508(9)
Li1 0.0425(16) 0.0282(15) 0.0285(15) -0.0054(12) -0.0083(12) -0.0168(13)
Li2 0.0410(15) 0.0219(13) 0.0173(12) 0.0001(10) -0.0089(11) -0.0112(11)

_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 1.9402(10) . ?
Cu1 O2 1.9331(11) . ?
Cu1 O11 1.9362(11) . ?
Cu1 O12 1.9286(11) . ?
Cu1 O1W 2.3705(14) . ?
C1 O1 1.2739(18) . ?
C1 O3 1.2442(18) . ?
C1 C2 1.509(2) . ?
C2 H1 0.90(2) . ?
C2 H2 0.92(2) . ?
C2 C3 1.515(2) . ?
C3 O2 1.2712(18) . ?
C3 O4 1.2377(18) . ?
C11 O11 1.2699(18) . ?
C11 O13 1.2458(18) . ?
C11 C12 1.514(2) . ?
C12 H11 0.92(2) . ?
C12 H12 0.97(2) . ?
C12 C13 1.510(2) . ?
C13 O12 1.2801(18) . ?
C13 O14 1.2295(19) . ?
O1W H1W1 0.67(3) . ?
O1W H2W1 0.76(3) . ?
O2W H1W2 0.73(3) . ?
O2W H2W2 0.77(3) . ?
O3W H1W3 0.74(3) . ?
O3W H2W3 0.78(3) . ?
Li1 O1 2.146(3) . ?
Li1 O12 2.057(3) . ?
Li1 O1W 2.096(3) 2_566 ?
Li1 O2W 1.969(3) . ?
Li1 O2W 2.055(3) 2_666 ?
Li2 O3 1.914(3) . ?
Li2 O3W 1.873(3) . ?
Li2 O13 1.962(3) 2_656 ?
Li2 O13 1.999(3) 1_556 ?

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 O1 93.14(5) . . ?
O12 Cu1 O11 94.32(5) . . ?
O11 Cu1 O1 158.85(5) . . ?
O12 Cu1 O2 174.69(5) . . ?
O12 Cu1 O1 82.33(4) . . ?
O2 Cu1 O11 88.91(5) . . ?
O1 Cu1 O1W 95.16(6) . . ?
O2 Cu1 O1W 95.03(5) . . ?
O11 Cu1 O1W 105.63(6) . . ?
O12 Cu1 O1W 88.16(5) . . ?
O3 C1 O1 122.24(13) . . ?
O3 C1 C2 119.18(13) . . ?
O1 C1 C2 118.55(13) . . ?
C1 C2 C3 116.06(13) . . ?
C1 C2 H1 111.0(12) . . ?
C3 C2 H1 109.5(13) . . ?
C1 C2 H2 105.5(13) . . ?
C3 C2 H2 106.7(13) . . ?
H1 C2 H2 107.6(17) . . ?
O4 C3 O2 122.55(14) . . ?
O4 C3 C2 117.06(13) . . ?
O2 C3 C2 120.38(13) . . ?
C1 O1 Cu1 126.01(9) . . ?
C1 O1 Li1 134.77(12) . . ?
Cu1 O1 Li1 98.97(9) . . ?
C3 O2 Cu1 125.26(10) . . ?
C1 O3 Li2 126.26(13) . . ?
O13 C11 O11 122.19(14) . . ?
O13 C11 C12 117.30(13) . . ?
O11 C11 C12 120.46(13) . . ?
C13 C12 C11 117.85(13) . . ?
C13 C12 H11 107.9(14) . . ?
C11 C12 H11 110.2(14) . . ?
C13 C12 H12 105.1(13) . . ?
C11 C12 H12 105.9(14) . . ?
H11 C12 H12 109.5(19) . . ?
O14 C13 O12 121.62(14) . . ?
O14 C13 C12 119.53(14) . . ?
O12 C13 C12 118.76(13) . . ?
C11 O11 Cu1 126.12(10) . . ?
C13 O12 Cu1 128.55(10) . . ?
C13 O12 Li1 122.18(13) . . ?
Cu1 O12 Li1 102.50(10) . . ?
C11 O13 Li2 136.57(13) . 2_656 ?
C11 O13 Li2 124.83(13) . 1_554 ?
Li2 O13 Li2 90.57(12) 2_656 1_554 ?
Li1 O1W Cu1 109.18(10) 2_566 . ?
Li1 O1W H1W1 120(3) 2_566 . ?
Cu1 O1W H1W1 114(3) . . ?
Li1 O1W H2W1 95(2) 2_566 . ?
Cu1 O1W H2W1 109(2) . . ?
H1W1 O1W H2W1 108(3) . . ?
Li1 O2W Li1 90.32(13) . 2_666 ?
Li1 O2W H1W2 107.8(19) . . ?
Li1 O2W H1W2 113.5(19) 2_666 . ?
Li1 O2W H2W2 127.1(16) . . ?
Li1 O2W H2W2 112.4(16) 2_666 . ?
H1W2 O2W H2W2 105(2) . . ?
Li2 O3W H1W3 123(2) . . ?
Li2 O3W H2W3 126.5(18) . . ?
H1W3 O3W H2W3 110(3) . . ?
O2W Li1 O1 88.55(13) . . ?
O12 Li1 O1W 99.87(14) . 2_566 ?
O1W Li1 O1 152.76(17) 2_566 . ?
O2W Li1 O12 163.04(18) . . ?
O12 Li1 O1 74.54(10) . . ?
O2W Li1 O1W 95.78(14) . 2_566 ?
O2W Li1 O1 109.58(15) 2_666 . ?
O2W Li1 O12 94.72(13) 2_666 . ?
O2W Li1 O1W 97.35(13) 2_666 2_566 ?
O2W Li1 O2W 89.68(13) . 2_666 ?
O3W Li2 O3 112.28(15) . . ?
O3 Li2 O13 112.84(14) . 2_656 ?
O3W Li2 O13 115.80(16) . 2_656 ?
O3 Li2 O13 121.92(16) . 1_556 ?
O3W Li2 O13 102.79(13) . 1_556 ?
O13 Li2 O13 89.43(12) 2_656 1_556 ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.050

# Attachment 'compound2.cif'

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 256112'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H8 Cu Na2 O10'
_chemical_formula_weight         349.64

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'
Na Na 0.0362 0.0249 '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           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_Int_Tables_number      61

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

_cell_length_a                   6.8270(10)
_cell_length_b                   9.517(2)
_cell_length_c                   16.406(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1065.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             700
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_type   'Multi-scan sadabs'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5136
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         5.24
_diffrn_reflns_theta_max         30.00
_reflns_number_total             1547
_reflns_number_gt                1071
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.0334P)^2^+0.8022P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1547
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0740
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_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 0.0000 0.5000 0.0000 0.01621(12) Uani 1 2 d S . .
Na1 Na 0.00032(17) 0.36203(11) 0.20010(6) 0.0240(2) Uani 1 1 d . . .
C1 C 0.1003(4) 0.2059(2) 0.01817(14) 0.0159(5) Uani 1 1 d . . .
C2 C 0.0632(4) 0.1917(3) -0.07283(15) 0.0161(5) Uani 1 1 d . . .
C3 C 0.1296(4) 0.3113(2) -0.12660(15) 0.0158(5) Uani 1 1 d . . .
O1 O 0.0524(3) 0.32095(19) 0.05402(10) 0.0195(4) Uani 1 1 d . . .
O2 O 0.1079(3) 0.43838(18) -0.10384(10) 0.0184(4) Uani 1 1 d . . .
O3 O 0.1732(3) 0.10505(19) 0.05410(11) 0.0249(4) Uani 1 1 d . . .
O4 O 0.1994(3) 0.27979(19) -0.19456(11) 0.0259(5) Uani 1 1 d . . .
O1W O 0.2972(3) 0.4893(2) 0.20747(13) 0.0243(4) Uani 1 1 d . . .
H1W1 H 0.284(5) 0.552(4) 0.238(2) 0.027(9) Uiso 1 1 d . . .
H1 H 0.116(5) 0.108(3) -0.0893(18) 0.022(8) Uiso 1 1 d . . .
H2W1 H 0.318(6) 0.524(4) 0.165(3) 0.036(10) Uiso 1 1 d . . .
H2 H -0.065(6) 0.182(4) -0.081(2) 0.038(10) Uiso 1 1 d . . .

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 0.0246(2) 0.01229(19) 0.01175(18) -0.00010(15) 0.00339(19) 0.00352(18)
Na1 0.0250(6) 0.0259(5) 0.0212(5) -0.0017(4) 0.0023(5) -0.0034(5)
C1 0.0153(13) 0.0154(11) 0.0169(11) 0.0009(9) 0.0002(9) -0.0012(9)
C2 0.0203(12) 0.0131(11) 0.0148(11) -0.0015(9) 0.0000(9) 0.0008(10)
C3 0.0162(11) 0.0169(11) 0.0143(10) -0.0006(9) -0.0019(9) 0.0024(9)
O1 0.0290(10) 0.0151(8) 0.0144(8) 0.0000(7) 0.0005(7) 0.0047(7)
O2 0.0263(10) 0.0142(8) 0.0146(8) -0.0010(7) 0.0051(7) 0.0013(7)
O3 0.0355(12) 0.0179(9) 0.0211(9) 0.0054(8) -0.0008(8) 0.0077(8)
O4 0.0414(13) 0.0201(9) 0.0162(9) -0.0007(7) 0.0097(8) 0.0072(8)
O1W 0.0360(12) 0.0210(10) 0.0159(9) 0.0012(8) -0.0005(8) -0.0016(9)

_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 1.9464(17) 5_565 ?
Cu1 O2 1.9464(17) . ?
Cu1 O1 1.9538(18) 5_565 ?
Cu1 O1 1.9538(18) . ?
Cu1 O3 2.601(2) 4_455 ?
Cu1 O3 2.601(2) 8_665 ?
Na1 O1W 2.364(2) . ?
Na1 O1W 2.385(2) 6_556 ?
Na1 O1 2.454(2) . ?
Na1 O4 2.460(2) 4_455 ?
Na1 O2 2.578(2) 5_565 ?
Na1 O4 2.580(2) 7_566 ?
C1 O1 1.285(3) . ?
C1 O3 1.232(3) . ?
C1 C2 1.520(3) . ?
C2 C3 1.509(3) . ?
C3 O2 1.275(3) . ?
C3 O4 1.249(3) . ?
O2 Na1 2.578(2) 5_565 ?
O4 Na1 2.460(2) 4 ?
O4 Na1 2.580(2) 7_565 ?
O1W Na1 2.385(2) 6_656 ?

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 180 5_565 . ?
O2 Cu1 O1 93.72(7) 5_565 5_565 ?
O2 Cu1 O1 86.28(7) . 5_565 ?
O2 Cu1 O1 86.28(7) 5_565 . ?
O2 Cu1 O1 93.72(7) . . ?
O1 Cu1 O1 180 5_565 . ?
O3 Cu1 O1 88.67(7) 4_455 . ?
O3 Cu1 O2 84.84(7) 4_455 . ?
O3 Cu1 O1 91.33(7) 4_455 5_565 ?
O3 Cu1 O2 95.16(7) 4_455 5_565 ?
O3 Cu1 O3 180 4_455 8_665 ?
O3 Cu1 O1 91.33(7) 8_665 . ?
O3 Cu1 O2 95.16(7) 8_665 . ?
O3 Cu1 O1 88.67(7) 8_665 5_565 ?
O3 Cu1 O2 84.84(7) 8_665 5_565 ?
O1W Na1 O1W 101.88(8) . 6_556 ?
O1W Na1 O1 90.42(8) . . ?
O1W Na1 O1 141.81(9) 6_556 . ?
O1W Na1 O4 177.43(9) . 4_455 ?
O1W Na1 O4 79.43(8) 6_556 4_455 ?
O1 Na1 O4 89.86(7) . 4_455 ?
O1W Na1 O2 84.23(7) . 5_565 ?
O1W Na1 O2 81.30(7) 6_556 5_565 ?
O1 Na1 O2 63.95(6) . 5_565 ?
O4 Na1 O2 98.19(7) 4_455 5_565 ?
O1W Na1 O4 77.42(8) . 7_566 ?
O1W Na1 O4 98.40(8) 6_556 7_566 ?
O1 Na1 O4 119.63(7) . 7_566 ?
O4 Na1 O4 100.23(7) 4_455 7_566 ?
O2 Na1 O4 161.20(8) 5_565 7_566 ?
O3 C1 O1 123.2(2) . . ?
O3 C1 C2 117.9(2) . . ?
O1 C1 C2 118.9(2) . . ?
C3 C2 C1 117.2(2) . . ?
O4 C3 O2 122.2(2) . . ?
O4 C3 C2 117.1(2) . . ?
O2 C3 C2 120.6(2) . . ?
C1 O1 Cu1 125.59(15) . . ?
C1 O1 Na1 128.29(15) . . ?
Cu1 O1 Na1 106.11(8) . . ?
C3 O2 Cu1 125.90(16) . . ?
C3 O2 Na1 123.58(15) . 5_565 ?
Cu1 O2 Na1 101.87(7) . 5_565 ?
C3 O4 Na1 118.89(17) . 4 ?
C3 O4 Na1 121.50(18) . 7_565 ?
Na1 O4 Na1 97.36(7) 4 7_565 ?
Na1 O1W Na1 105.71(9) . 6_656 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.092

# Attachment 'compound3.cif'

data_compound3
_database_code_depnum_ccdc_archive 'CCDC 256113'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H10 Cu K2 O11'
_chemical_formula_weight         399.88

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_Int_Tables_number      60

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

_cell_length_a                   7.3985(7)
_cell_length_b                   18.830(2)
_cell_length_c                   9.3201(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1298.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             804
_exptl_absorpt_coefficient_mu    2.376
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8013
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         6.46
_diffrn_reflns_theta_max         29.12
_reflns_number_total             1683
_reflns_number_gt                1187
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.0461P)^2^+0.7063P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0116(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         1683
_refine_ls_number_parameters     102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0889
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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 0.0000 -0.300253(17) 0.2500 0.02987(18) Uani 1 2 d S . .
K1 K 0.0000 -0.09363(4) 0.2500 0.0298(2) Uani 1 2 d S . .
K2 K 0.0000 -0.50166(4) 0.2500 0.0448(3) Uani 1 2 d S . .
C1 C 0.1426(3) -0.23438(10) 0.5039(2) 0.0220(5) Uani 1 1 d . . .
C2 C 0.1125(4) -0.30531(11) 0.5761(2) 0.0244(5) Uani 1 1 d . . .
C3 C 0.1610(3) -0.37094(11) 0.4909(2) 0.0245(5) Uani 1 1 d . . .
O1 O 0.0944(2) -0.22600(8) 0.37361(16) 0.0292(4) Uani 1 1 d . . .
O2 O 0.1207(2) -0.37422(8) 0.35872(15) 0.0288(4) Uani 1 1 d . . .
O3 O 0.2117(3) -0.18658(8) 0.57635(18) 0.0367(5) Uani 1 1 d . . .
O4 O 0.2352(3) -0.42036(9) 0.55588(19) 0.0428(5) Uani 1 1 d . . .
O1W O 0.0000 0.05421(17) 0.2500 0.0737(11) Uani 1 2 d S . .
O2W O -0.2296(3) -0.55791(9) 0.0564(2) 0.0438(5) Uani 1 1 d . . .
H1 H -0.015(4) -0.3074(12) 0.591(3) 0.029(7) Uiso 1 1 d . . .
H2 H 0.180(3) -0.3059(11) 0.665(3) 0.019(6) Uiso 1 1 d . . .

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 0.0543(3) 0.0144(2) 0.0209(2) 0.000 -0.01628(18) 0.000
K1 0.0317(4) 0.0283(4) 0.0293(4) 0.000 0.0063(3) 0.000
K2 0.0667(6) 0.0230(4) 0.0447(5) 0.000 -0.0178(4) 0.000
C1 0.0288(13) 0.0179(10) 0.0191(10) -0.0031(8) -0.0004(9) -0.0004(9)
C2 0.0338(14) 0.0232(10) 0.0160(10) 0.0013(8) -0.0019(10) -0.0015(10)
C3 0.0289(13) 0.0195(9) 0.0250(11) 0.0018(8) -0.0063(9) -0.0011(9)
O1 0.0490(11) 0.0184(7) 0.0201(8) 0.0010(6) -0.0089(7) -0.0034(7)
O2 0.0474(10) 0.0203(7) 0.0189(8) -0.0016(6) -0.0095(7) 0.0034(7)
O3 0.0578(12) 0.0251(8) 0.0272(9) -0.0054(7) -0.0095(8) -0.0101(8)
O4 0.0675(14) 0.0254(8) 0.0355(10) 0.0005(8) -0.0246(9) 0.0099(9)
O1W 0.104(3) 0.0392(16) 0.077(2) 0.000 -0.014(2) 0.000
O2W 0.0552(13) 0.0324(10) 0.0437(11) -0.0008(8) -0.0081(9) -0.0014(9)

_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 1.9400(15) 4 ?
Cu1 O2 1.9400(15) . ?
Cu1 O1 1.9417(15) . ?
Cu1 O1 1.9417(15) 4 ?
Cu1 O3 2.689(2) 2_544 ?
Cu1 O3 2.689(2) 3_446 ?
K1 O4 2.6795(18) 2_544 ?
K1 O4 2.6795(18) 3_446 ?
K1 O2W 2.777(2) 6_666 ?
K1 O2W 2.777(2) 7_565 ?
K1 O1W 2.784(3) . ?
K1 O1 2.8334(16) 4 ?
K1 O1 2.8334(16) . ?
K2 O2W 2.6947(19) . ?
K2 O2W 2.6947(19) 4 ?
K2 O2 2.7535(16) . ?
K2 O2 2.7535(16) 4 ?
K2 O4 2.908(2) 5_546 ?
K2 O4 2.908(2) 8_545 ?
C1 O1 1.275(2) . ?
C1 O3 1.236(2) . ?
C1 C2 1.512(3) . ?
C2 C3 1.512(3) . ?
C3 O2 1.269(3) . ?
C3 O4 1.239(3) . ?
O4 K1 2.6795(18) 2_545 ?
O4 K2 2.908(2) 5_546 ?
O2W K1 2.777(2) 6_556 ?

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 88.23(9) 4 . ?
O2 Cu1 O1 172.95(7) 4 . ?
O2 Cu1 O1 92.38(6) . . ?
O2 Cu1 O1 92.38(6) 4 4 ?
O2 Cu1 O1 172.95(7) . 4 ?
O1 Cu1 O1 87.88(9) . 4 ?
O3 Cu1 O1 97.94(6) 2_544 . ?
O3 Cu1 O2 83.29(6) 2_544 . ?
O3 Cu1 O1 89.70(6) 2_544 4 ?
O3 Cu1 O2 89.11(6) 2_544 4 ?
O3 Cu1 O3 169.42(6) 2_544 3_446 ?
O3 Cu1 O1 89.70(6) 3_446 . ?
O3 Cu1 O2 89.11(6) 3_446 . ?
O3 Cu1 O1 97.94(6) 3_446 4 ?
O3 Cu1 O2 83.29(6) 3_446 4 ?
O4 K1 O4 168.71(8) 2_544 3_446 ?
O4 K1 O2W 83.57(6) 2_544 6_666 ?
O4 K1 O2W 93.68(6) 3_446 6_666 ?
O4 K1 O2W 93.68(6) 2_544 7_565 ?
O4 K1 O2W 83.57(6) 3_446 7_565 ?
O2W K1 O2W 151.96(8) 6_666 7_565 ?
O4 K1 O1W 84.36(4) 2_544 . ?
O4 K1 O1W 84.36(4) 3_446 . ?
O2W K1 O1W 75.98(4) 6_666 . ?
O2W K1 O1W 75.98(4) 7_565 . ?
O4 K1 O1 89.56(5) 2_544 4 ?
O4 K1 O1 100.41(5) 3_446 4 ?
O2W K1 O1 130.92(5) 6_666 4 ?
O2W K1 O1 76.78(5) 7_565 4 ?
O1W K1 O1 151.61(3) . 4 ?
O4 K1 O1 100.41(5) 2_544 . ?
O4 K1 O1 89.56(5) 3_446 . ?
O2W K1 O1 76.78(5) 6_666 . ?
O2W K1 O1 130.92(5) 7_565 . ?
O1W K1 O1 151.61(3) . . ?
O1 K1 O1 56.79(6) 4 . ?
O2W K2 O2W 133.71(8) . 4 ?
O2W K2 O2 142.49(5) . . ?
O2W K2 O2 83.79(5) 4 . ?
O2W K2 O2 83.79(5) . 4 ?
O2W K2 O2 142.49(5) 4 4 ?
O2 K2 O2 58.74(6) . 4 ?
O2W K2 O4 80.84(6) . 5_546 ?
O2W K2 O4 76.24(6) 4 5_546 ?
O2 K2 O4 113.90(5) . 5_546 ?
O2 K2 O4 118.35(5) 4 5_546 ?
O2W K2 O4 76.24(6) . 8_545 ?
O2W K2 O4 80.84(6) 4 8_545 ?
O2 K2 O4 118.35(5) . 8_545 ?
O2 K2 O4 113.90(5) 4 8_545 ?
O4 K2 O4 119.35(8) 5_546 8_545 ?
O3 C1 O1 123.07(19) . . ?
O3 C1 C2 117.47(19) . . ?
O1 C1 C2 119.45(17) . . ?
C1 C2 C3 116.96(18) . . ?
O4 C3 O2 122.9(2) . . ?
O4 C3 C2 117.55(19) . . ?
O2 C3 C2 119.56(18) . . ?
C1 O1 Cu1 125.20(13) . . ?
C1 O1 K1 124.40(12) . . ?
Cu1 O1 K1 107.66(6) . . ?
C3 O2 Cu1 125.48(14) . . ?
C3 O2 K2 118.42(13) . . ?
Cu1 O2 K2 106.52(6) . . ?
C3 O4 K1 125.47(15) . 2_545 ?
C3 O4 K2 114.73(17) . 5_546 ?
K1 O4 K2 93.85(5) 2_545 5_546 ?
K2 O2W K1 96.57(6) . 6_556 ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        29.12
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.068

# Attachment 'compound4.cif'

data_compound4
_database_code_depnum_ccdc_archive 'CCDC 256114'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H6 Cu O9 Rb2'
_chemical_formula_weight         456.59

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'
Cu Cu 0.3201 1.2651 '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'
Rb Rb -0.9393 2.9676 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_Int_Tables_number      19

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

_cell_length_a                   7.2224(6)
_cell_length_b                   9.4647(5)
_cell_length_c                   17.017(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1163.25(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       sheet
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             868
_exptl_absorpt_coefficient_mu    10.228
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   '(SADABS, Sheldrick, 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  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5038
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.19
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2318
_reflns_number_gt                1671
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.0448P)^2^+1.4026P] 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   0.49(2)
_refine_ls_number_reflns         2318
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.1037
_refine_ls_wR_factor_gt          0.0936
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
Rb1 Rb -0.21804(13) -0.00953(8) -0.05621(6) 0.0310(2) Uani 1 1 d . . .
Rb2 Rb 0.21218(13) -0.04866(9) -0.43943(5) 0.0287(2) Uani 1 1 d . . .
Cu1 Cu 0.26900(16) -0.01424(9) -0.19181(7) 0.0264(3) Uani 1 1 d . . .
C1 C 0.3730(14) 0.2550(9) -0.2527(6) 0.024(2) Uani 1 1 d . . .
C2 C 0.3512(12) 0.3120(8) -0.1700(6) 0.025(2) Uani 1 1 d . . .
H1 H 0.4223 0.3986 -0.1661 0.029 Uiso 1 1 calc R . .
H2 H 0.2221 0.3366 -0.1623 0.029 Uiso 1 1 calc R . .
C3 C 0.4083(12) 0.2175(11) -0.1040(6) 0.024(2) Uani 1 1 d . . .
O1 O 0.3418(9) 0.1273(6) -0.2683(4) 0.0342(18) Uani 1 1 d . . .
O2 O 0.3876(9) 0.0857(6) -0.1074(4) 0.0277(15) Uani 1 1 d . . .
O4 O 0.4712(10) 0.2736(7) -0.0426(4) 0.0383(19) Uani 1 1 d . . .
O3 O 0.4287(9) 0.3389(6) -0.3051(4) 0.0359(18) Uani 1 1 d . . .
C11 C 0.1302(13) -0.2549(9) -0.2752(6) 0.023(2) Uani 1 1 d . . .
C12 C 0.1594(12) -0.3367(8) -0.2000(6) 0.028(2) Uani 1 1 d . . .
H12 H 0.2884 -0.3652 -0.1980 0.034 Uiso 1 1 calc R . .
H11 H 0.0860 -0.4223 -0.2031 0.034 Uiso 1 1 calc R . .
C13 C 0.1133(13) -0.2638(9) -0.1226(5) 0.020(2) Uani 1 1 d . . .
O11 O 0.1661(9) -0.1219(6) -0.2766(4) 0.0312(17) Uani 1 1 d . . .
O12 O 0.1486(9) -0.1319(6) -0.1156(4) 0.0289(16) Uani 1 1 d . . .
O13 O 0.0760(10) -0.3179(6) -0.3332(5) 0.040(2) Uani 1 1 d . . .
O14 O 0.0520(11) -0.3359(7) -0.0687(5) 0.042(2) Uani 1 1 d . . .
O1W O 0.0132(10) -0.1651(7) 0.0605(5) 0.0434(19) Uani 1 1 d . . .

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
Rb1 0.0325(5) 0.0323(4) 0.0284(5) 0.0093(4) 0.0019(5) 0.0017(5)
Rb2 0.0320(5) 0.0297(4) 0.0245(5) -0.0004(4) -0.0005(5) 0.0094(4)
Cu1 0.0470(7) 0.0205(5) 0.0116(5) 0.0017(4) -0.0017(5) -0.0115(5)
C1 0.034(6) 0.026(5) 0.013(6) 0.003(4) 0.005(4) -0.002(4)
C2 0.027(5) 0.021(4) 0.026(6) -0.004(4) -0.002(4) 0.002(4)
C3 0.017(5) 0.039(5) 0.017(6) -0.001(5) 0.009(4) -0.001(5)
O1 0.061(5) 0.024(3) 0.017(4) 0.004(3) 0.002(3) -0.008(3)
O2 0.048(4) 0.020(3) 0.015(4) 0.000(3) -0.007(3) -0.003(3)
O4 0.055(5) 0.044(4) 0.016(5) 0.003(3) -0.006(4) -0.027(4)
O3 0.050(4) 0.030(3) 0.028(5) 0.010(3) 0.004(4) -0.006(3)
C11 0.022(5) 0.036(6) 0.010(5) -0.006(4) 0.001(4) 0.012(4)
C12 0.028(6) 0.017(4) 0.040(7) 0.001(4) 0.001(5) -0.005(4)
C13 0.019(5) 0.028(5) 0.013(5) 0.003(4) -0.009(4) -0.009(4)
O11 0.053(5) 0.025(3) 0.016(4) 0.001(3) -0.008(3) -0.004(3)
O12 0.047(4) 0.023(3) 0.017(4) 0.005(3) 0.006(3) -0.011(3)
O13 0.064(5) 0.035(4) 0.022(5) -0.011(3) -0.005(4) 0.002(4)
O14 0.069(5) 0.042(4) 0.015(5) 0.009(4) -0.001(4) -0.029(4)
O1W 0.056(5) 0.041(4) 0.033(5) 0.005(4) 0.001(5) -0.001(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
Rb1 O13 2.808(7) 4_554 ?
Rb1 O1W 2.984(8) . ?
Rb1 O12 3.062(6) . ?
Rb1 O14 3.069(8) 3_445 ?
Rb1 O4 3.112(8) 3_455 ?
Rb1 O2 3.112(6) 1_455 ?
Rb1 O3 3.154(7) 4_544 ?
Rb2 O14 2.778(6) 4_554 ?
Rb2 O1W 2.833(7) 2_554 ?
Rb2 O4 2.855(6) 4_644 ?
Rb2 O11 2.876(7) . ?
Rb2 O2 2.968(7) 2_554 ?
Rb2 O4 3.061(6) 2_554 ?
Rb2 O13 3.276(7) . ?
Cu1 O11 1.916(6) . ?
Cu1 O12 1.917(6) . ?
Cu1 O2 1.922(6) . ?
Cu1 O1 1.941(6) . ?
C1 O1 1.258(10) . ?
C1 O3 1.260(11) . ?
C1 C2 1.516(13) . ?
C2 C3 1.493(13) . ?
C2 H1 0.9700 . ?
C2 H2 0.9700 . ?
C3 O2 1.258(11) . ?
C3 O4 1.257(11) . ?
O2 Rb2 2.968(7) 2 ?
O2 Rb1 3.112(6) 1_655 ?
O4 Rb2 2.855(6) 4_654 ?
O4 Rb2 3.061(6) 2 ?
O4 Rb1 3.112(8) 3 ?
O3 Rb1 3.154(7) 4_554 ?
C11 O11 1.286(10) . ?
C11 O13 1.218(11) . ?
C11 C12 1.510(13) . ?
C12 C13 1.524(13) . ?
C12 H12 0.9700 . ?
C12 H11 0.9700 . ?
C13 O12 1.279(10) . ?
C13 O14 1.226(11) . ?
O13 Rb1 2.808(7) 4_544 ?
O14 Rb2 2.778(6) 4_544 ?
O14 Rb1 3.069(8) 3_545 ?
O1W Rb2 2.833(7) 2 ?

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
O13 Rb1 O1W 124.1(2) 4_554 . ?
O13 Rb1 O12 72.96(18) 4_554 . ?
O1W Rb1 O12 63.2(2) . . ?
O13 Rb1 O14 165.9(2) 4_554 3_445 ?
O1W Rb1 O14 66.83(18) . 3_445 ?
O12 Rb1 O14 121.09(17) . 3_445 ?
O13 Rb1 O4 74.8(2) 4_554 3_455 ?
O1W Rb1 O4 75.44(18) . 3_455 ?
O12 Rb1 O4 94.02(17) . 3_455 ?
O14 Rb1 O4 101.9(2) 3_445 3_455 ?
O13 Rb1 O2 87.69(19) 4_554 1_455 ?
O1W Rb1 O2 147.31(19) . 1_455 ?
O12 Rb1 O2 143.98(19) . 1_455 ?
O14 Rb1 O2 80.59(18) 3_445 1_455 ?
O4 Rb1 O2 110.20(16) 3_455 1_455 ?
O13 Rb1 O3 88.17(19) 4_554 4_544 ?
O1W Rb1 O3 122.95(18) . 4_544 ?
O12 Rb1 O3 89.89(17) . 4_544 ?
O14 Rb1 O3 92.32(19) 3_445 4_544 ?
O4 Rb1 O3 160.54(16) 3_455 4_544 ?
O2 Rb1 O3 58.72(16) 1_455 4_544 ?
O14 Rb2 O1W 87.88(19) 4_554 2_554 ?
O14 Rb2 O4 169.3(2) 4_554 4_644 ?
O1W Rb2 O4 82.0(2) 2_554 4_644 ?
O14 Rb2 O11 92.7(2) 4_554 . ?
O1W Rb2 O11 104.7(2) 2_554 . ?
O4 Rb2 O11 93.09(18) 4_644 . ?
O14 Rb2 O2 88.1(2) 4_554 2_554 ?
O1W Rb2 O2 104.7(2) 2_554 2_554 ?
O4 Rb2 O2 91.25(18) 4_644 2_554 ?
O11 Rb2 O2 150.61(16) . 2_554 ?
O14 Rb2 O4 103.6(2) 4_554 2_554 ?
O1W Rb2 O4 143.1(2) 2_554 2_554 ?
O4 Rb2 O4 82.84(8) 4_644 2_554 ?
O11 Rb2 O4 109.59(18) . 2_554 ?
O2 Rb2 O4 42.30(17) 2_554 2_554 ?
O14 Rb2 O13 109.3(2) 4_554 . ?
O1W Rb2 O13 140.0(2) 2_554 . ?
O4 Rb2 O13 80.86(19) 4_644 . ?
O11 Rb2 O13 41.06(17) . . ?
O2 Rb2 O13 111.51(17) 2_554 . ?
O4 Rb2 O13 69.25(17) 2_554 . ?
O11 Cu1 O12 91.4(3) . . ?
O11 Cu1 O2 176.0(3) . . ?
O12 Cu1 O2 89.0(3) . . ?
O11 Cu1 O1 88.1(3) . . ?
O12 Cu1 O1 167.8(3) . . ?
O2 Cu1 O1 92.4(3) . . ?
O1 C1 O3 120.9(9) . . ?
O1 C1 C2 121.3(8) . . ?
O3 C1 C2 117.8(7) . . ?
C3 C2 C1 117.2(7) . . ?
C3 C2 H1 108.0 . . ?
C1 C2 H1 108.0 . . ?
C3 C2 H2 108.0 . . ?
C1 C2 H2 108.0 . . ?
H1 C2 H2 107.2 . . ?
O4 C3 O2 120.0(9) . . ?
O4 C3 C2 118.1(9) . . ?
O2 C3 C2 121.8(8) . . ?
C1 O1 Cu1 124.7(6) . . ?
C3 O2 Cu1 125.1(6) . . ?
C3 O2 Rb2 95.9(5) . 2 ?
Cu1 O2 Rb2 123.6(3) . 2 ?
C3 O2 Rb1 99.5(6) . 1_655 ?
Cu1 O2 Rb1 118.3(3) . 1_655 ?
Rb2 O2 Rb1 85.33(16) 2 1_655 ?
C3 O4 Rb2 116.7(6) . 4_654 ?
C3 O4 Rb2 91.5(6) . 2 ?
Rb2 O4 Rb2 144.8(3) 4_654 2 ?
C3 O4 Rb1 126.4(6) . 3 ?
Rb2 O4 Rb1 89.24(18) 4_654 3 ?
Rb2 O4 Rb1 89.95(19) 2 3 ?
C3 O4 Rb1 81.6(6) . 1_655 ?
Rb2 O4 Rb1 86.01(19) 4_654 1_655 ?
Rb2 O4 Rb1 77.46(15) 2 1_655 ?
Rb1 O4 Rb1 150.0(2) 3 1_655 ?
C1 O3 Rb1 131.5(6) . 4_554 ?
O13 C11 O11 121.9(9) . . ?
O13 C11 C12 118.7(8) . . ?
O11 C11 C12 119.3(8) . . ?
C11 C12 C13 118.0(7) . . ?
C11 C12 H12 107.8 . . ?
C13 C12 H12 107.8 . . ?
C11 C12 H11 107.8 . . ?
C13 C12 H11 107.8 . . ?
H12 C12 H11 107.1 . . ?
O14 C13 O12 123.1(9) . . ?
O14 C13 C12 118.2(8) . . ?
O12 C13 C12 118.6(8) . . ?
C11 O11 Cu1 125.8(6) . . ?
C11 O11 Rb2 106.1(5) . . ?
Cu1 O11 Rb2 123.5(3) . . ?
C13 O12 Cu1 126.5(6) . . ?
C13 O12 Rb1 103.1(5) . . ?
Cu1 O12 Rb1 113.3(3) . . ?
C11 O13 Rb1 137.9(6) . 4_544 ?
C11 O13 Rb2 88.3(6) . . ?
Rb1 O13 Rb2 91.3(2) 4_544 . ?
C13 O14 Rb2 133.5(7) . 4_544 ?
C13 O14 Rb1 126.0(6) . 3_545 ?
Rb2 O14 Rb1 89.51(19) 4_544 3_545 ?
Rb2 O1W Rb1 92.3(2) 2 . ?

_diffrn_measured_fraction_theta_max 0.937
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.937
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.183

# Attachment 'compound5.cif'

data_compound5
_database_code_depnum_ccdc_archive 'CCDC 256115'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H8 Cs Cu O6'
_chemical_formula_weight         336.54

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'
Cs Cs -0.3680 2.1192 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.1166(6)
_cell_length_b                   7.1316(9)
_cell_length_c                   7.5211(6)
_cell_angle_alpha                87.334(8)
_cell_angle_beta                 79.428(7)
_cell_angle_gamma                86.698(8)
_cell_volume                     374.36(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       sheet
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             316
_exptl_absorpt_coefficient_mu    7.690
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3756
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         6.46
_diffrn_reflns_theta_max         27.49
_reflns_number_total             1681
_reflns_number_gt                1523
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.0395P)^2^+0.1310P] 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         1681
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0790
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_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 0.5000 0.0000 0.0000 0.01853(16) Uani 1 2 d S . .
Cs1 Cs 0.29659(4) -0.26027(3) 0.49325(3) 0.03082(12) Uani 1 1 d . . .
C1 C 0.3353(5) 0.3712(5) -0.0640(5) 0.0198(7) Uani 1 1 d . . .
C2 C 0.2074(6) 0.3499(6) 0.1179(6) 0.0277(8) Uani 1 1 d . . .
H1 H 0.0982 0.2810 0.1024 0.033 Uiso 1 1 calc R . .
H2 H 0.1592 0.4743 0.1564 0.033 Uiso 1 1 calc R . .
C3 C 0.2938(6) 0.2525(5) 0.2692(5) 0.0216(7) Uani 1 1 d . . .
O1 O 0.4370(4) 0.2295(4) -0.1287(4) 0.0267(6) Uani 1 1 d . . .
O2 O 0.4022(4) 0.1064(3) 0.2383(4) 0.0248(6) Uani 1 1 d . . .
O3 O 0.3315(5) 0.5225(4) -0.1493(4) 0.0334(7) Uani 1 1 d . . .
O4 O 0.2487(5) 0.3193(4) 0.4235(4) 0.0389(8) Uani 1 1 d . . .
O1W O 0.2027(4) -0.1362(4) -0.0218(4) 0.0307(6) Uani 1 1 d . . .
O2W O -0.0743(5) -0.1052(5) 0.2882(5) 0.0421(8) Uani 1 1 d . . .

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 0.0264(3) 0.0152(3) 0.0129(3) 0.0009(2) -0.0021(2) 0.0027(2)
Cs1 0.04271(19) 0.02697(17) 0.02093(17) 0.00158(11) -0.00280(11) 0.00234(11)
C1 0.0270(18) 0.0179(16) 0.0162(17) -0.0023(13) -0.0088(14) 0.0008(13)
C2 0.030(2) 0.0282(19) 0.023(2) -0.0027(16) -0.0017(16) 0.0075(16)
C3 0.0275(18) 0.0179(16) 0.0173(18) -0.0006(14) 0.0024(14) -0.0050(14)
O1 0.0394(16) 0.0220(13) 0.0152(13) 0.0028(11) 0.0008(11) 0.0053(11)
O2 0.0377(15) 0.0195(12) 0.0165(13) -0.0021(10) -0.0042(11) 0.0029(11)
O3 0.056(2) 0.0171(12) 0.0257(16) 0.0031(11) -0.0074(14) 0.0052(12)
O4 0.062(2) 0.0322(16) 0.0182(15) -0.0052(13) 0.0019(14) 0.0049(14)
O1W 0.0301(15) 0.0234(14) 0.0372(18) -0.0010(12) -0.0025(13) -0.0009(11)
O2W 0.0403(18) 0.054(2) 0.0295(17) 0.0020(15) -0.0033(14) 0.0004(16)

_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 1.935(3) . ?
Cu1 O1 1.935(3) 2_655 ?
Cu1 O2 1.970(3) 2_655 ?
Cu1 O2 1.970(3) . ?
Cu1 O1W 2.414(3) . ?
Cu1 O1W 2.414(3) 2_655 ?
Cs1 O1 3.040(3) 2_655 ?
Cs1 O3 3.083(3) 1_546 ?
Cs1 O4 3.117(3) 1_545 ?
Cs1 O2 3.211(3) . ?
Cs1 O2W 3.311(4) 2_556 ?
Cs1 O2W 3.401(3) . ?
Cs1 O4 3.407(4) 2_656 ?
Cs1 O2 3.456(3) 2_656 ?
Cs1 O1W 3.724(3) 1_556 ?
C1 O3 1.231(4) . ?
C1 O1 1.270(5) . ?
C1 C2 1.504(6) . ?
C2 C3 1.514(5) . ?
C3 O4 1.254(5) . ?
C3 O2 1.264(5) . ?
O1 Cs1 3.040(3) 2_655 ?
O2 Cs1 3.456(3) 2_656 ?
O3 Cs1 3.083(3) 1_564 ?
O4 Cs1 3.117(3) 1_565 ?
O4 Cs1 3.407(4) 2_656 ?
O1W Cs1 3.724(3) 1_554 ?
O2W Cs1 3.311(4) 2_556 ?

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 180.00(19) . 2_655 ?
O1 Cu1 O2 87.18(11) . 2_655 ?
O1 Cu1 O2 92.82(11) 2_655 2_655 ?
O1 Cu1 O2 92.82(11) . . ?
O1 Cu1 O2 87.18(11) 2_655 . ?
O2 Cu1 O2 180.00(17) 2_655 . ?
O1 Cu1 O1W 92.90(11) . . ?
O1 Cu1 O1W 87.10(11) 2_655 . ?
O2 Cu1 O1W 85.50(11) 2_655 . ?
O2 Cu1 O1W 94.50(11) . . ?
O1 Cu1 O1W 87.10(11) . 2_655 ?
O1 Cu1 O1W 92.90(11) 2_655 2_655 ?
O2 Cu1 O1W 94.50(11) 2_655 2_655 ?
O2 Cu1 O1W 85.50(11) . 2_655 ?
O1W Cu1 O1W 180.00(11) . 2_655 ?
O1 Cs1 O3 132.82(8) 2_655 1_546 ?
O1 Cs1 O4 88.97(8) 2_655 1_545 ?
O3 Cs1 O4 74.25(8) 1_546 1_545 ?
O1 Cs1 O2 50.94(7) 2_655 . ?
O3 Cs1 O2 146.99(7) 1_546 . ?
O4 Cs1 O2 134.55(7) 1_545 . ?
O1 Cs1 O2W 123.91(7) 2_655 2_556 ?
O3 Cs1 O2W 91.86(8) 1_546 2_556 ?
O4 Cs1 O2W 142.24(9) 1_545 2_556 ?
O2 Cs1 O2W 73.05(8) . 2_556 ?
O1 Cs1 O2W 88.96(8) 2_655 . ?
O3 Cs1 O2W 134.78(8) 1_546 . ?
O4 Cs1 O2W 93.43(9) 1_545 . ?
O2 Cs1 O2W 68.82(8) . . ?
O2W Cs1 O2W 71.48(10) 2_556 . ?
O1 Cs1 O4 73.33(7) 2_655 2_656 ?
O3 Cs1 O4 65.40(8) 1_546 2_656 ?
O4 Cs1 O4 96.22(8) 1_545 2_656 ?
O2 Cs1 O4 91.77(7) . 2_656 ?
O2W Cs1 O4 109.82(8) 2_556 2_656 ?
O2W Cs1 O4 159.61(8) . 2_656 ?
O1 Cs1 O2 98.65(7) 2_655 2_656 ?
O3 Cs1 O2 60.62(7) 1_546 2_656 ?
O4 Cs1 O2 124.59(7) 1_545 2_656 ?
O2 Cs1 O2 86.64(6) . 2_656 ?
O2W Cs1 O2 72.72(7) 2_556 2_656 ?
O2W Cs1 O2 141.11(8) . 2_656 ?
O4 Cs1 O2 37.57(7) 2_656 2_656 ?
O1 Cs1 O1W 146.62(7) 2_655 1_556 ?
O3 Cs1 O1W 45.65(7) 1_546 1_556 ?
O4 Cs1 O1W 115.17(7) 1_545 1_556 ?
O2 Cs1 O1W 110.26(6) . 1_556 ?
O2W Cs1 O1W 46.90(7) 2_556 1_556 ?
O2W Cs1 O1W 110.87(8) . 1_556 ?
O4 Cs1 O1W 81.05(7) 2_656 1_556 ?
O2 Cs1 O1W 49.10(6) 2_656 1_556 ?
C3 Cs1 O1W 61.41(8) 2_656 1_556 ?
O3 C1 O1 122.0(4) . . ?
O3 C1 C2 119.1(3) . . ?
O1 C1 C2 118.9(3) . . ?
C1 C2 C3 117.3(3) . . ?
O4 C3 O2 122.7(4) . . ?
O4 C3 C2 117.4(4) . . ?
O2 C3 C2 119.9(3) . . ?
C1 O1 Cu1 127.4(2) . . ?
C1 O1 Cs1 120.8(2) . 2_655 ?
Cu1 O1 Cs1 109.94(11) . 2_655 ?
C3 O2 Cu1 126.5(2) . . ?
C3 O2 Cs1 117.4(2) . . ?
Cu1 O2 Cs1 102.83(9) . . ?
C3 O2 Cs1 90.6(2) . 2_656 ?
Cu1 O2 Cs1 122.12(12) . 2_656 ?
Cs1 O2 Cs1 93.36(6) . 2_656 ?
C1 O3 Cs1 148.8(2) . 1_564 ?
C3 O4 Cs1 122.4(2) . 1_565 ?
C3 O4 Cs1 93.0(3) . 2_656 ?
Cs1 O4 Cs1 83.78(8) 1_565 2_656 ?
Cu1 O1W Cs1 100.78(10) . 1_554 ?
Cs1 O2W Cs1 108.52(10) 2_556 . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.739
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.174


