# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Hongjie Zhang'
_publ_contact_author_email       HONGJIE@CIAC.JL.CN

_publ_section_title              
;
Tetracarboxylate-based Co(II), Ni(II) and Cu(II)
three-dimensional porous coordination polymers:
syntheses, structures and magnetic properties
;
loop_
_publ_author_name
'Hongjie Zhang'
'Feng Cao'
'Ruiping Deng'
'Zhiyong Guo'
'Huadong Guo'
;
Guanghua Li
;
'Cheng-Ling Pan'
'Shu-Yan Song'
'Shengqun Su'
'Song Wang'

# Attachment '1.cif'

data_aa
_database_code_depnum_ccdc_archive 'CCDC 763322'
#TrackingRef '1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C40 H36 Co3 N2 O20'
_chemical_formula_sum            'C40 H36 Co3 N2 O20'
_chemical_formula_weight         1041.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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                   16.223(3)
_cell_length_b                   10.633(2)
_cell_length_c                   25.188(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4345.0(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    4263
_cell_measurement_theta_min      1.62
_cell_measurement_theta_max      26.01

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2124
_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6847
_exptl_absorpt_correction_T_max  0.7228
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            22619
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         26.01
_reflns_number_total             4263
_reflns_number_gt                3697
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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^)+(0.0301P)^2^+0.9072P] 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         4263
_refine_ls_number_parameters     241
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0232
_refine_ls_wR_factor_ref         0.0600
_refine_ls_wR_factor_gt          0.0589
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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
Co1 Co 0.062909(12) 0.344015(19) 0.381262(8) 0.01292(7) Uani 1 1 d . . .
Co2 Co 0.0000 0.5000 0.5000 0.01086(8) Uani 1 2 d S . .
O1 O 0.10356(6) 0.43945(10) 0.45219(4) 0.0161(2) Uani 1 1 d . . .
O2 O 0.17903(7) 0.29135(11) 0.41767(4) 0.0235(3) Uani 1 1 d . . .
O3 O 0.43837(6) 0.16612(10) 0.51183(4) 0.0173(2) Uani 1 1 d . . .
O4 O 0.48156(7) 0.27372(10) 0.58301(4) 0.0219(3) Uani 1 1 d . . .
O5 O 0.45369(7) 0.91691(10) 0.56758(4) 0.0188(2) Uani 1 1 d . . .
O6 O 0.48620(8) 1.01692(11) 0.64307(4) 0.0262(3) Uani 1 1 d . . .
O7 O 0.44237(7) 0.76840(10) 0.81340(4) 0.0205(3) Uani 1 1 d . . .
O8 O 0.36238(8) 0.60379(12) 0.80963(4) 0.0292(3) Uani 1 1 d . . .
C1 C 0.23143(9) 0.39212(14) 0.49575(6) 0.0155(3) Uani 1 1 d . . .
C2 C 0.30123(10) 0.31717(14) 0.49935(6) 0.0175(3) Uani 1 1 d . . .
H2 H 0.3110 0.2552 0.4741 0.080 Uiso 1 1 calc . . .
C3 C 0.35679(9) 0.33507(14) 0.54107(6) 0.0162(3) Uani 1 1 d . . .
C4 C 0.33956(9) 0.42441(14) 0.58028(6) 0.0163(3) Uani 1 1 d . . .
H4 H 0.3756 0.4341 0.6087 0.080 Uiso 1 1 calc . . .
C5 C 0.26933(9) 0.49878(13) 0.57731(6) 0.0147(3) Uani 1 1 d . . .
C6 C 0.21763(9) 0.48496(14) 0.53366(6) 0.0148(3) Uani 1 1 d . . .
H6 H 0.1729 0.5389 0.5297 0.080 Uiso 1 1 calc . . .
C7 C 0.24146(9) 0.58343(14) 0.62226(6) 0.0169(3) Uani 1 1 d . . .
H7A H 0.1999 0.6403 0.6085 0.080 Uiso 1 1 calc . . .
H7B H 0.2150 0.5314 0.6489 0.080 Uiso 1 1 calc . . .
C8 C 0.30685(9) 0.66107(14) 0.64936(6) 0.0145(3) Uani 1 1 d . . .
C9 C 0.35170(9) 0.75188(14) 0.62182(6) 0.0153(3) Uani 1 1 d . . .
H9 H 0.3444 0.7601 0.5854 0.080 Uiso 1 1 calc . . .
C10 C 0.40705(9) 0.83032(14) 0.64783(6) 0.0151(3) Uani 1 1 d . . .
C11 C 0.42015(10) 0.81534(14) 0.70237(6) 0.0163(3) Uani 1 1 d . . .
H11 H 0.4569 0.8677 0.7201 0.080 Uiso 1 1 calc . . .
C12 C 0.37797(9) 0.72175(14) 0.72996(6) 0.0164(3) Uani 1 1 d . . .
C13 C 0.32103(10) 0.64713(14) 0.70344(6) 0.0171(3) Uani 1 1 d . . .
H13 H 0.2918 0.5866 0.7223 0.080 Uiso 1 1 calc . . .
C14 C 0.16872(9) 0.37240(14) 0.45314(6) 0.0151(3) Uani 1 1 d . . .
C15 C 0.43189(9) 0.25180(14) 0.54538(6) 0.0147(3) Uani 1 1 d . . .
C16 C 0.45326(10) 0.92912(14) 0.61681(6) 0.0160(3) Uani 1 1 d . . .
C17 C 0.39444(10) 0.69655(15) 0.78732(6) 0.0171(3) 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
Co1 0.01185(11) 0.01681(11) 0.01010(11) -0.00200(8) -0.00046(8) -0.00010(8)
Co2 0.01035(14) 0.01338(14) 0.00886(14) -0.00090(11) -0.00078(10) -0.00028(11)
O1 0.0132(5) 0.0215(6) 0.0136(5) -0.0031(4) -0.0028(4) 0.0021(4)
O2 0.0184(6) 0.0325(6) 0.0195(6) -0.0127(5) -0.0043(5) 0.0058(5)
O3 0.0145(6) 0.0171(5) 0.0202(6) -0.0042(5) -0.0023(4) 0.0034(4)
O4 0.0223(6) 0.0235(6) 0.0198(6) -0.0055(5) -0.0095(5) 0.0075(5)
O5 0.0188(6) 0.0256(6) 0.0120(6) 0.0028(5) 0.0019(4) -0.0043(5)
O6 0.0375(7) 0.0248(6) 0.0163(6) -0.0014(5) 0.0040(5) -0.0140(5)
O7 0.0269(6) 0.0230(6) 0.0117(5) 0.0022(4) -0.0055(5) -0.0068(5)
O8 0.0348(7) 0.0354(7) 0.0174(6) 0.0113(5) -0.0057(5) -0.0140(6)
C1 0.0139(8) 0.0189(7) 0.0138(7) 0.0002(6) -0.0010(6) -0.0011(6)
C2 0.0174(8) 0.0195(8) 0.0156(8) -0.0046(6) 0.0000(6) 0.0008(6)
C3 0.0148(8) 0.0166(7) 0.0172(8) -0.0005(6) -0.0008(6) 0.0007(6)
C4 0.0139(8) 0.0186(8) 0.0165(8) 0.0001(6) -0.0027(6) -0.0007(6)
C5 0.0160(8) 0.0144(7) 0.0136(7) 0.0004(6) -0.0002(6) -0.0025(6)
C6 0.0119(7) 0.0163(7) 0.0161(7) 0.0009(6) 0.0005(6) -0.0001(6)
C7 0.0144(8) 0.0196(8) 0.0166(8) -0.0054(6) -0.0012(6) 0.0002(6)
C8 0.0135(8) 0.0142(7) 0.0157(8) -0.0027(6) -0.0003(6) 0.0032(6)
C9 0.0173(8) 0.0176(7) 0.0109(7) -0.0015(6) -0.0001(6) 0.0030(6)
C10 0.0162(8) 0.0152(7) 0.0139(8) 0.0003(6) 0.0011(6) 0.0022(6)
C11 0.0178(8) 0.0173(8) 0.0140(8) -0.0007(6) -0.0007(6) -0.0007(6)
C12 0.0173(8) 0.0182(8) 0.0136(7) 0.0003(6) -0.0003(6) -0.0011(6)
C13 0.0177(8) 0.0175(8) 0.0159(8) 0.0001(6) 0.0013(6) -0.0022(6)
C14 0.0129(8) 0.0196(8) 0.0129(7) 0.0005(6) -0.0002(6) -0.0007(6)
C15 0.0139(8) 0.0150(7) 0.0151(8) 0.0023(6) -0.0003(6) 0.0000(6)
C16 0.0155(8) 0.0176(8) 0.0151(8) 0.0017(6) 0.0021(6) 0.0020(6)
C17 0.0180(8) 0.0211(8) 0.0123(8) 0.0012(6) -0.0007(6) 0.0004(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
Co1 O6 2.0276(11) 4_466 ?
Co1 O4 2.0295(11) 4_456 ?
Co1 O7 2.0876(11) 2_564 ?
Co1 O1 2.1580(11) . ?
Co1 O2 2.1687(12) . ?
Co1 O8 2.2432(12) 2_564 ?
Co1 C17 2.5028(16) 2_564 ?
Co1 C14 2.5131(15) . ?
Co2 O3 2.0515(11) 8_665 ?
Co2 O3 2.0515(11) 4_456 ?
Co2 O5 2.0598(11) 4_466 ?
Co2 O5 2.0598(11) 8_655 ?
Co2 O1 2.1650(11) . ?
Co2 O1 2.1650(11) 5_566 ?
O1 C14 1.2752(18) . ?
O2 C14 1.2527(18) . ?
O3 C15 1.2471(18) . ?
O3 Co2 2.0515(11) 4_556 ?
O4 C15 1.2658(18) . ?
O4 Co1 2.0295(11) 4_556 ?
O5 C16 1.2467(18) . ?
O5 Co2 2.0598(11) 4_566 ?
O6 C16 1.2628(19) . ?
O6 Co1 2.0276(11) 4_566 ?
O7 C17 1.2728(19) . ?
O7 Co1 2.0876(11) 2_565 ?
O8 C17 1.249(2) . ?
O8 Co1 2.2432(12) 2_565 ?
C1 C2 1.388(2) . ?
C1 C6 1.392(2) . ?
C1 C14 1.494(2) . ?
C2 C3 1.397(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.399(2) . ?
C3 C15 1.510(2) . ?
C4 C5 1.389(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.391(2) . ?
C5 C7 1.515(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.508(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C13 1.390(2) . ?
C8 C9 1.394(2) . ?
C9 C10 1.390(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.399(2) . ?
C10 C16 1.509(2) . ?
C11 C12 1.393(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.389(2) . ?
C12 C17 1.494(2) . ?
C13 H13 0.9300 . ?
C17 Co1 2.5028(16) 2_565 ?

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
O6 Co1 O4 100.65(5) 4_466 4_456 ?
O6 Co1 O7 98.33(5) 4_466 2_564 ?
O4 Co1 O7 89.03(4) 4_456 2_564 ?
O6 Co1 O1 95.45(4) 4_466 . ?
O4 Co1 O1 96.99(4) 4_456 . ?
O7 Co1 O1 163.68(4) 2_564 . ?
O6 Co1 O2 148.14(5) 4_466 . ?
O4 Co1 O2 102.60(5) 4_456 . ?
O7 Co1 O2 103.53(4) 2_564 . ?
O1 Co1 O2 60.39(4) . . ?
O6 Co1 O8 84.72(5) 4_466 2_564 ?
O4 Co1 O8 149.38(4) 4_456 2_564 ?
O7 Co1 O8 60.35(4) 2_564 2_564 ?
O1 Co1 O8 112.61(4) . 2_564 ?
O2 Co1 O8 86.25(5) . 2_564 ?
O6 Co1 C17 90.55(5) 4_466 2_564 ?
O4 Co1 C17 119.52(5) 4_456 2_564 ?
O7 Co1 C17 30.52(5) 2_564 2_564 ?
O1 Co1 C17 141.20(5) . 2_564 ?
O2 Co1 C17 96.61(5) . 2_564 ?
O8 Co1 C17 29.87(5) 2_564 2_564 ?
O6 Co1 C14 123.33(5) 4_466 . ?
O4 Co1 C14 101.47(5) 4_456 . ?
O7 Co1 C14 133.37(5) 2_564 . ?
O1 Co1 C14 30.49(4) . . ?
O2 Co1 C14 29.90(4) . . ?
O8 Co1 C14 100.41(5) 2_564 . ?
C17 Co1 C14 120.86(5) 2_564 . ?
O3 Co2 O3 180.00(6) 8_665 4_456 ?
O3 Co2 O5 85.90(4) 8_665 4_466 ?
O3 Co2 O5 94.10(4) 4_456 4_466 ?
O3 Co2 O5 94.10(4) 8_665 8_655 ?
O3 Co2 O5 85.90(4) 4_456 8_655 ?
O5 Co2 O5 180.00(3) 4_466 8_655 ?
O3 Co2 O1 87.63(4) 8_665 . ?
O3 Co2 O1 92.37(4) 4_456 . ?
O5 Co2 O1 87.19(4) 4_466 . ?
O5 Co2 O1 92.81(4) 8_655 . ?
O3 Co2 O1 92.37(4) 8_665 5_566 ?
O3 Co2 O1 87.63(4) 4_456 5_566 ?
O5 Co2 O1 92.81(4) 4_466 5_566 ?
O5 Co2 O1 87.19(4) 8_655 5_566 ?
O1 Co2 O1 180.0 . 5_566 ?
C14 O1 Co1 90.34(9) . . ?
C14 O1 Co2 143.04(10) . . ?
Co1 O1 Co2 111.29(5) . . ?
C14 O2 Co1 90.45(9) . . ?
C15 O3 Co2 140.22(10) . 4_556 ?
C15 O4 Co1 129.23(10) . 4_556 ?
C16 O5 Co2 141.20(11) . 4_566 ?
C16 O6 Co1 129.83(10) . 4_566 ?
C17 O7 Co1 93.08(9) . 2_565 ?
C17 O8 Co1 86.65(9) . 2_565 ?
C2 C1 C6 119.59(14) . . ?
C2 C1 C14 121.48(13) . . ?
C6 C1 C14 118.89(13) . . ?
C1 C2 C3 119.82(14) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C2 C3 C4 119.65(14) . . ?
C2 C3 C15 119.65(13) . . ?
C4 C3 C15 120.57(13) . . ?
C5 C4 C3 120.84(14) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 118.50(13) . . ?
C4 C5 C7 122.87(13) . . ?
C6 C5 C7 118.26(13) . . ?
C5 C6 C1 121.36(14) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
C8 C7 C5 116.97(13) . . ?
C8 C7 H7A 108.1 . . ?
C5 C7 H7A 108.1 . . ?
C8 C7 H7B 108.1 . . ?
C5 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
C13 C8 C9 118.39(14) . . ?
C13 C8 C7 120.13(14) . . ?
C9 C8 C7 121.41(13) . . ?
C10 C9 C8 121.22(14) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 119.52(14) . . ?
C9 C10 C16 119.66(14) . . ?
C11 C10 C16 120.81(14) . . ?
C12 C11 C10 119.76(14) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C13 C12 C11 119.66(14) . . ?
C13 C12 C17 118.79(14) . . ?
C11 C12 C17 121.52(14) . . ?
C12 C13 C8 121.37(14) . . ?
C12 C13 H13 119.3 . . ?
C8 C13 H13 119.3 . . ?
O2 C14 O1 118.82(13) . . ?
O2 C14 C1 121.21(13) . . ?
O1 C14 C1 119.97(13) . . ?
O2 C14 Co1 59.65(8) . . ?
O1 C14 Co1 59.17(7) . . ?
C1 C14 Co1 178.83(11) . . ?
O3 C15 O4 126.04(14) . . ?
O3 C15 C3 116.59(13) . . ?
O4 C15 C3 117.36(13) . . ?
O5 C16 O6 126.55(15) . . ?
O5 C16 C10 116.45(14) . . ?
O6 C16 C10 116.99(13) . . ?
O8 C17 O7 119.76(14) . . ?
O8 C17 C12 120.18(14) . . ?
O7 C17 C12 120.06(14) . . ?
O8 C17 Co1 63.48(8) . 2_565 ?
O7 C17 Co1 56.40(8) . 2_565 ?
C12 C17 Co1 174.25(11) . 2_565 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.048

# Attachment '2.CIF'

data_aaa
_database_code_depnum_ccdc_archive 'CCDC 763323'
#TrackingRef '2.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C20 H39 N Ni2 O21'
_chemical_formula_sum            'C20 H39 N Ni2 O21'
_chemical_formula_weight         746.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.247(2)
_cell_length_b                   15.250(3)
_cell_length_c                   20.946(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.91(3)
_cell_angle_gamma                90.00
_cell_volume                     3224.4(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    6313
_cell_measurement_theta_min      1.66
_cell_measurement_theta_max      26.08

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5362
_exptl_absorpt_correction_T_max  0.6819
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            17261
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         26.08
_reflns_number_total             6313
_reflns_number_gt                5587
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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^)+(0.0000P)^2^+63.7889P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6313
_refine_ls_number_parameters     382
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0818
_refine_ls_wR_factor_ref         0.2023
_refine_ls_wR_factor_gt          0.2008
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.109
_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
Ni1 Ni 0.25327(8) 0.26181(5) 0.33127(4) 0.0117(2) Uani 1 1 d . . .
Ni2 Ni 0.20295(8) 0.14291(5) 0.18574(4) 0.0122(2) Uani 1 1 d . . .
C1 C 0.4830(6) 0.0217(4) 0.3380(3) 0.0132(13) Uani 1 1 d . . .
C2 C 0.5496(7) 0.0323(4) 0.4017(3) 0.0143(13) Uani 1 1 d . . .
H2 H 0.5292 0.0799 0.4260 0.080 Uiso 1 1 calc . . .
C3 C 0.6460(6) -0.0272(4) 0.4293(3) 0.0120(13) Uani 1 1 d . . .
C4 C 0.6737(6) -0.0975(4) 0.3922(3) 0.0149(13) Uani 1 1 d . . .
H4 H 0.7366 -0.1385 0.4103 0.080 Uiso 1 1 calc . . .
C5 C 0.6099(7) -0.1083(4) 0.3287(3) 0.0147(13) Uani 1 1 d . . .
C6 C 0.5140(7) -0.0478(5) 0.3012(3) 0.0163(14) Uani 1 1 d . . .
H6 H 0.4715 -0.0544 0.2585 0.080 Uiso 1 1 calc . . .
C7 C 0.7231(7) -0.0110(5) 0.4963(3) 0.0149(14) Uani 1 1 d . . .
H7A H 0.7662 -0.0651 0.5128 0.080 Uiso 1 1 calc . . .
H7B H 0.6621 0.0056 0.5249 0.080 Uiso 1 1 calc . . .
C8 C 0.8287(6) 0.0613(4) 0.4976(3) 0.0128(13) Uani 1 1 d . . .
C9 C 0.8688(7) 0.1079(5) 0.5552(3) 0.0153(14) Uani 1 1 d . . .
H9 H 0.8326 0.0949 0.5919 0.080 Uiso 1 1 calc . . .
C10 C 0.9646(7) 0.1747(5) 0.5572(3) 0.0169(14) Uani 1 1 d . . .
C11 C 1.0183(6) 0.1936(4) 0.5026(3) 0.0137(13) Uani 1 1 d . . .
H11 H 1.0804 0.2384 0.5037 0.080 Uiso 1 1 calc . . .
C12 C 0.9792(7) 0.1454(4) 0.4454(3) 0.0134(13) Uani 1 1 d . . .
C13 C 0.8841(7) 0.0804(5) 0.4439(3) 0.0170(14) Uani 1 1 d . . .
H13 H 0.8572 0.0491 0.4058 0.080 Uiso 1 1 calc . . .
C14 C 0.3819(7) 0.0886(4) 0.3088(3) 0.0129(13) Uani 1 1 d . . .
C15 C 1.0115(7) 0.2240(5) 0.6187(3) 0.0169(14) Uani 1 1 d . . .
C16 C 1.0443(7) 0.1653(4) 0.3878(3) 0.0149(14) Uani 1 1 d . . .
C17 C 0.6486(6) -0.1843(4) 0.2895(3) 0.0145(14) Uani 1 1 d . . .
C18 C 0.4247(8) 0.2714(5) 0.4583(4) 0.0228(16) Uani 1 1 d . . .
H18 H 0.3923 0.2147 0.4604 0.080 Uiso 1 1 calc . . .
C19 C 0.5678(11) 0.3873(7) 0.5075(5) 0.047(3) Uani 1 1 d . . .
H19A H 0.6298 0.3961 0.5469 0.080 Uiso 1 1 calc . . .
H19B H 0.4982 0.4300 0.5047 0.080 Uiso 1 1 calc . . .
H19C H 0.6126 0.3937 0.4711 0.080 Uiso 1 1 calc . . .
C20 C 0.5532(10) 0.2456(7) 0.5642(5) 0.042(2) Uani 1 1 d . . .
H20A H 0.6174 0.2774 0.5943 0.080 Uiso 1 1 calc . . .
H20B H 0.5921 0.1922 0.5520 0.080 Uiso 1 1 calc . . .
H20C H 0.4781 0.2320 0.5843 0.080 Uiso 1 1 calc . . .
O1 O 0.3296(5) 0.0748(3) 0.2502(2) 0.0227(11) Uani 1 1 d . . .
O2 O 0.3644(5) 0.1530(3) 0.3431(2) 0.0201(11) Uani 1 1 d . . .
O3 O 0.9920(6) 0.1901(4) 0.6707(2) 0.0251(12) Uani 1 1 d . . .
H3 H 1.0218 0.2223 0.7011 0.080 Uiso 1 1 calc . . .
O4 O 1.0694(5) 0.2960(3) 0.6137(2) 0.0176(10) Uani 1 1 d . . .
O5 O 1.1422(5) 0.2151(3) 0.3968(2) 0.0165(10) Uani 1 1 d . . .
O6 O 0.9923(5) 0.1309(3) 0.3344(2) 0.0218(11) Uani 1 1 d . . .
O7 O 0.6793(5) -0.2528(3) 0.3209(2) 0.0214(11) Uani 1 1 d . . .
O8 O 0.6474(5) -0.1720(3) 0.2301(2) 0.0185(10) Uani 1 1 d . . .
O9 O 0.1187(5) 0.2077(3) 0.2556(2) 0.0147(10) Uani 1 1 d D . .
H9A H 0.046(8) 0.181(8) 0.271(6) 0.080 Uiso 1 1 d D . .
O10 O 0.3817(5) 0.3154(3) 0.4085(2) 0.0214(11) Uani 1 1 d . . .
O11 O 0.1463(5) 0.3770(3) 0.3334(3) 0.0213(11) Uani 1 1 d D . .
O12 O 0.2842(5) 0.0763(4) 0.1162(3) 0.0249(12) Uani 1 1 d D . .
O13 O 0.0678(5) 0.0415(3) 0.1808(3) 0.0234(11) Uani 1 1 d D . .
N1 N 0.5109(6) 0.2986(4) 0.5073(3) 0.0234(14) Uani 1 1 d . . .
O1W O 0.0509(8) 0.4722(4) 0.2219(3) 0.0442(18) Uani 1 1 d . . .
O2W O 0.2052(8) 0.4268(5) 0.4847(3) 0.052(2) Uani 1 1 d . . .
O3W O 0.4569(8) 0.4905(6) 0.3550(3) 0.059(2) Uani 1 1 d . . .
O4W O 0.0875(9) 0.5907(6) 0.4812(4) 0.066(2) Uani 1 1 d . . .
H11A H 0.142(12) 0.409(6) 0.295(3) 0.080 Uiso 1 1 d D . .
H11B H 0.191(11) 0.406(6) 0.372(3) 0.080 Uiso 1 1 d D . .
H12A H 0.284(11) 0.059(7) 0.0705(17) 0.080 Uiso 1 1 d D . .
H12B H 0.353(9) 0.041(7) 0.144(4) 0.080 Uiso 1 1 d D . .
H13A H 0.010(9) 0.047(8) 0.140(3) 0.080 Uiso 1 1 d D . .
H13B H 0.021(9) 0.012(8) 0.210(4) 0.080 Uiso 1 1 d 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
Ni1 0.0141(4) 0.0097(4) 0.0116(4) 0.0004(3) 0.0031(3) 0.0001(3)
Ni2 0.0154(4) 0.0101(4) 0.0111(4) 0.0007(3) 0.0020(3) 0.0001(3)
C1 0.009(3) 0.017(3) 0.013(3) 0.001(3) 0.001(2) -0.001(3)
C2 0.016(3) 0.014(3) 0.012(3) -0.001(3) -0.001(3) -0.001(3)
C3 0.014(3) 0.014(3) 0.008(3) 0.002(2) 0.003(2) -0.004(3)
C4 0.012(3) 0.017(3) 0.016(3) 0.002(3) 0.003(3) 0.001(3)
C5 0.015(3) 0.015(3) 0.013(3) -0.002(3) 0.001(3) 0.001(3)
C6 0.016(3) 0.016(3) 0.015(3) -0.001(3) -0.005(3) 0.001(3)
C7 0.016(3) 0.021(4) 0.007(3) 0.002(3) -0.002(2) -0.007(3)
C8 0.010(3) 0.014(3) 0.013(3) 0.003(3) -0.002(2) -0.002(3)
C9 0.021(3) 0.016(3) 0.010(3) 0.000(3) 0.005(3) -0.001(3)
C10 0.020(3) 0.015(3) 0.015(3) -0.003(3) 0.000(3) -0.004(3)
C11 0.011(3) 0.013(3) 0.016(3) -0.001(3) 0.000(3) -0.005(2)
C12 0.017(3) 0.014(3) 0.009(3) 0.002(2) 0.002(3) 0.001(3)
C13 0.017(3) 0.019(3) 0.014(3) -0.003(3) 0.000(3) -0.003(3)
C14 0.020(3) 0.013(3) 0.007(3) 0.001(2) 0.005(3) 0.002(3)
C15 0.017(3) 0.017(3) 0.017(3) -0.005(3) 0.005(3) 0.000(3)
C16 0.021(3) 0.013(3) 0.011(3) -0.001(2) 0.003(3) -0.003(3)
C17 0.005(3) 0.018(3) 0.020(4) -0.004(3) 0.000(2) -0.002(2)
C18 0.026(4) 0.023(4) 0.020(4) -0.003(3) 0.004(3) 0.000(3)
C19 0.055(6) 0.036(5) 0.045(6) -0.008(4) -0.007(5) -0.021(5)
C20 0.042(5) 0.054(6) 0.029(5) 0.009(4) 0.000(4) -0.011(5)
O1 0.028(3) 0.017(3) 0.020(3) -0.004(2) -0.007(2) 0.011(2)
O2 0.024(3) 0.019(3) 0.016(2) -0.003(2) 0.000(2) 0.008(2)
O3 0.038(3) 0.027(3) 0.010(2) -0.007(2) 0.005(2) -0.016(2)
O4 0.021(2) 0.018(2) 0.013(2) 0.0013(19) 0.0007(19) -0.006(2)
O5 0.017(2) 0.018(2) 0.014(2) 0.0006(19) 0.0031(19) -0.004(2)
O6 0.029(3) 0.023(3) 0.013(2) -0.003(2) 0.004(2) -0.009(2)
O7 0.032(3) 0.014(2) 0.020(3) 0.004(2) 0.010(2) 0.010(2)
O8 0.025(3) 0.019(3) 0.013(2) 0.0003(19) 0.006(2) 0.005(2)
O9 0.014(2) 0.014(2) 0.016(2) -0.0003(19) 0.0042(19) -0.0004(19)
O10 0.024(3) 0.019(3) 0.019(3) -0.004(2) 0.000(2) 0.000(2)
O11 0.025(3) 0.015(3) 0.024(3) 0.001(2) 0.005(2) 0.003(2)
O12 0.027(3) 0.031(3) 0.018(3) -0.005(2) 0.006(2) 0.006(2)
O13 0.023(3) 0.021(3) 0.025(3) 0.000(2) 0.003(2) -0.008(2)
N1 0.025(3) 0.026(3) 0.019(3) -0.002(3) 0.001(3) 0.000(3)
O1W 0.083(5) 0.029(3) 0.022(3) 0.008(3) 0.012(3) 0.016(3)
O2W 0.078(5) 0.053(4) 0.024(3) -0.004(3) 0.005(3) 0.022(4)
O3W 0.075(5) 0.073(5) 0.034(4) -0.018(4) 0.023(4) -0.042(5)
O4W 0.067(5) 0.060(5) 0.079(6) 0.024(5) 0.032(5) 0.023(4)

_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
Ni1 O2 2.003(5) . ?
Ni1 O8 2.039(5) 2_655 ?
Ni1 O5 2.056(5) 1_455 ?
Ni1 O10 2.069(5) . ?
Ni1 O11 2.075(5) . ?
Ni1 O9 2.084(5) . ?
Ni2 O1 1.997(5) . ?
Ni2 O7 2.016(5) 2_655 ?
Ni2 O12 2.066(5) . ?
Ni2 O13 2.067(5) . ?
Ni2 O9 2.074(5) . ?
Ni2 O4 2.075(5) 4_465 ?
C1 C6 1.380(10) . ?
C1 C2 1.400(9) . ?
C1 C14 1.506(9) . ?
C2 C3 1.392(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(9) . ?
C3 C7 1.508(9) . ?
C4 C5 1.388(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(9) . ?
C5 C17 1.512(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.543(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C13 1.376(9) . ?
C8 C9 1.400(9) . ?
C9 C10 1.411(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.384(10) . ?
C10 C15 1.496(9) . ?
C11 C12 1.404(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(10) . ?
C12 C16 1.506(9) . ?
C13 H13 0.9300 . ?
C14 O2 1.248(8) . ?
C14 O1 1.270(8) . ?
C15 O3 1.253(9) . ?
C15 O4 1.261(8) . ?
C16 O5 1.246(8) . ?
C16 O6 1.267(8) . ?
C17 O7 1.246(9) . ?
C17 O8 1.256(8) . ?
C18 O10 1.256(9) . ?
C18 N1 1.301(10) . ?
C18 H18 0.9300 . ?
C19 N1 1.473(11) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N1 1.445(11) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
O3 H3 0.8200 . ?
O4 Ni2 2.075(5) 4_666 ?
O5 Ni1 2.056(5) 1_655 ?
O7 Ni2 2.016(5) 2_645 ?
O8 Ni1 2.039(5) 2_645 ?
O9 H9A 0.95(2) . ?
O11 H11A 0.94(2) . ?
O11 H11B 0.95(2) . ?
O12 H12A 0.99(2) . ?
O12 H12B 0.99(2) . ?
O13 H13A 0.96(2) . ?
O13 H13B 0.95(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
O2 Ni1 O8 98.8(2) . 2_655 ?
O2 Ni1 O5 89.9(2) . 1_455 ?
O8 Ni1 O5 170.6(2) 2_655 1_455 ?
O2 Ni1 O10 87.6(2) . . ?
O8 Ni1 O10 88.7(2) 2_655 . ?
O5 Ni1 O10 88.0(2) 1_455 . ?
O2 Ni1 O11 171.7(2) . . ?
O8 Ni1 O11 85.3(2) 2_655 . ?
O5 Ni1 O11 85.6(2) 1_455 . ?
O10 Ni1 O11 85.2(2) . . ?
O2 Ni1 O9 93.11(19) . . ?
O8 Ni1 O9 93.07(19) 2_655 . ?
O5 Ni1 O9 90.04(19) 1_455 . ?
O10 Ni1 O9 177.9(2) . . ?
O11 Ni1 O9 93.9(2) . . ?
O1 Ni2 O7 97.5(2) . 2_655 ?
O1 Ni2 O12 85.8(2) . . ?
O7 Ni2 O12 91.2(2) 2_655 . ?
O1 Ni2 O13 89.8(2) . . ?
O7 Ni2 O13 172.3(2) 2_655 . ?
O12 Ni2 O13 86.8(2) . . ?
O1 Ni2 O9 94.1(2) . . ?
O7 Ni2 O9 89.9(2) 2_655 . ?
O12 Ni2 O9 178.8(2) . . ?
O13 Ni2 O9 92.0(2) . . ?
O1 Ni2 O4 175.0(2) . 4_465 ?
O7 Ni2 O4 85.6(2) 2_655 4_465 ?
O12 Ni2 O4 90.2(2) . 4_465 ?
O13 Ni2 O4 87.0(2) . 4_465 ?
O9 Ni2 O4 89.77(19) . 4_465 ?
C6 C1 C2 120.0(6) . . ?
C6 C1 C14 120.1(6) . . ?
C2 C1 C14 119.8(6) . . ?
C3 C2 C1 121.0(6) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C4 C3 C2 118.2(6) . . ?
C4 C3 C7 121.6(6) . . ?
C2 C3 C7 120.1(6) . . ?
C3 C4 C5 121.5(6) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C4 C5 C6 119.9(6) . . ?
C4 C5 C17 119.2(6) . . ?
C6 C5 C17 120.9(6) . . ?
C1 C6 C5 119.4(6) . . ?
C1 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C3 C7 C8 112.8(5) . . ?
C3 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
C3 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C13 C8 C9 119.8(6) . . ?
C13 C8 C7 121.6(6) . . ?
C9 C8 C7 118.6(6) . . ?
C8 C9 C10 119.4(6) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 120.1(6) . . ?
C11 C10 C15 119.5(6) . . ?
C9 C10 C15 120.4(6) . . ?
C10 C11 C12 120.0(6) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 119.3(6) . . ?
C13 C12 C16 122.1(6) . . ?
C11 C12 C16 118.5(6) . . ?
C8 C13 C12 121.3(6) . . ?
C8 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
O2 C14 O1 127.5(6) . . ?
O2 C14 C1 117.1(6) . . ?
O1 C14 C1 115.2(6) . . ?
O3 C15 O4 125.3(6) . . ?
O3 C15 C10 117.7(6) . . ?
O4 C15 C10 116.9(6) . . ?
O5 C16 O6 126.3(6) . . ?
O5 C16 C12 117.2(6) . . ?
O6 C16 C12 116.5(6) . . ?
O7 C17 O8 127.3(6) . . ?
O7 C17 C5 114.9(6) . . ?
O8 C17 C5 117.7(6) . . ?
O10 C18 N1 125.4(7) . . ?
O10 C18 H18 117.3 . . ?
N1 C18 H18 117.3 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 H20A 109.5 . . ?
N1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C14 O1 Ni2 133.2(4) . . ?
C14 O2 Ni1 135.7(5) . . ?
C15 O3 H3 109.5 . . ?
C15 O4 Ni2 126.3(4) . 4_666 ?
C16 O5 Ni1 129.3(4) . 1_655 ?
C17 O7 Ni2 136.5(5) . 2_645 ?
C17 O8 Ni1 129.0(4) . 2_645 ?
Ni2 O9 Ni1 115.1(2) . . ?
Ni2 O9 H9A 119(8) . . ?
Ni1 O9 H9A 112(8) . . ?
C18 O10 Ni1 121.6(5) . . ?
Ni1 O11 H11A 112(8) . . ?
Ni1 O11 H11B 103(7) . . ?
H11A O11 H11B 115(3) . . ?
Ni2 O12 H12A 151(6) . . ?
Ni2 O12 H12B 101(6) . . ?
H12A O12 H12B 108(3) . . ?
Ni2 O13 H13A 107(7) . . ?
Ni2 O13 H13B 137(7) . . ?
H13A O13 H13B 108(3) . . ?
C18 N1 C20 122.6(7) . . ?
C18 N1 C19 120.7(7) . . ?
C20 N1 C19 116.7(7) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 O9 0.82 1.74 2.546(7) 165.8 4_666
O9 H9A O6 0.95(2) 1.71(7) 2.551(7) 146(11) 1_455
O11 H11A O1W 0.94(2) 1.90(6) 2.782(8) 153(11) .
O11 H11B O2W 0.95(2) 2.37(6) 3.213(8) 147(9) .
O12 H12A O2W 0.99(2) 1.85(6) 2.734(8) 146(8) 4_565
O12 H12B O3W 0.99(2) 2.09(7) 2.926(9) 141(9) 2_645
O13 H13A O4W 0.96(2) 2.65(4) 3.571(11) 162(8) 2_545
O13 H13B O1W 0.95(2) 1.82(3) 2.757(8) 168(10) 2_545

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        26.08
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.034
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.169

# Attachment '3.cif'

data_sad
_database_code_depnum_ccdc_archive 'CCDC 763324'
#TrackingRef '3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C17 H31 Cu3 O20.50'
_chemical_formula_sum            'C17 H31 Cu3 O20.50'
_chemical_formula_weight         754.04

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           Orthorhombic
_symmetry_space_group_name_H-M   Pccn

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

_cell_length_a                   18.4609(10)
_cell_length_b                   18.6553(10)
_cell_length_c                   8.1387(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2802.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    2754
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      26.07

_exptl_crystal_description       rod
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5081
_exptl_absorpt_correction_T_max  0.5762
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            14433
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         26.07
_reflns_number_total             2754
_reflns_number_gt                2286
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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^)+(0.0771P)^2^+7.6753P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2754
_refine_ls_number_parameters     230
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1354
_refine_ls_wR_factor_gt          0.1272
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.061
_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 0.06924(3) 0.58564(3) 0.20933(7) 0.02394(19) Uani 1 1 d D . .
Cu2 Cu 0.0000 0.5000 0.5000 0.0249(2) Uani 1 2 d S . .
C1 C 0.2128(2) 0.42153(19) 0.2989(5) 0.0192(8) Uani 1 1 d . . .
C2 C 0.2822(2) 0.4415(2) 0.2542(5) 0.0194(8) Uani 1 1 d . . .
H2 H 0.2896 0.4833 0.1942 0.080 Uiso 1 1 calc . . .
C3 C 0.3410(2) 0.3993(2) 0.2990(5) 0.0175(7) Uani 1 1 d . . .
C4 C 0.3301(2) 0.33741(19) 0.3917(4) 0.0173(7) Uani 1 1 d . . .
H4 H 0.3696 0.3097 0.4230 0.080 Uiso 1 1 calc . . .
C5 C 0.2606(2) 0.31694(19) 0.4376(4) 0.0174(7) Uani 1 1 d . . .
C6 C 0.2021(2) 0.3586(2) 0.3891(5) 0.0192(8) Uani 1 1 d . . .
H6 H 0.1554 0.3445 0.4168 0.080 Uiso 1 1 calc . . .
C7 C 0.2500 0.2500 0.5402(6) 0.0203(11) Uani 1 2 d S . .
H7A H 0.2919 0.2435 0.6105 0.080 Uiso 0.50 1 calc P . .
H7B H 0.2081 0.2565 0.6105 0.080 Uiso 0.50 1 calc P . .
C8 C 0.1496(2) 0.4680(2) 0.2544(5) 0.0248(9) Uani 1 1 d . . .
C9 C 0.4164(2) 0.4202(2) 0.2502(5) 0.0204(8) Uani 1 1 d . . .
O1 O 0.08743(16) 0.44293(18) 0.2475(5) 0.0344(7) Uani 1 1 d . . .
O2 O 0.16322(16) 0.53457(15) 0.2273(4) 0.0314(7) Uani 1 1 d . . .
O3 O 0.42224(16) 0.47229(17) 0.1513(5) 0.0365(8) Uani 1 1 d . . .
O4 O 0.46729(16) 0.38477(17) 0.3078(4) 0.0289(7) Uani 1 1 d . . .
O5 O 0.05719(16) 0.58315(14) 0.4467(4) 0.0254(6) Uani 1 1 d D . .
H5 H 0.054(4) 0.629(2) 0.495(8) 0.080 Uiso 1 1 d D . .
O6 O 0.0742(2) 0.5877(3) -0.0362(6) 0.0646(13) Uani 1 1 d D . .
H6A H 0.045(3) 0.619(2) -0.100(8) 0.080 Uiso 1 1 d D . .
H6B H 0.058(3) 0.5408(14) -0.065(3) 0.080 Uiso 1 1 d D . .
O7 O 0.1208(2) 0.6989(2) 0.1984(5) 0.0534(10) Uani 1 1 d D . .
H7C H 0.092(3) 0.731(3) 0.143(7) 0.080 Uiso 1 1 d D . .
H7D H 0.137(4) 0.720(3) 0.295(5) 0.080 Uiso 1 1 d D . .
O1W O 0.0205(3) 0.7808(2) 0.0355(5) 0.0579(11) Uani 1 1 d . . .
O2W O 0.0456(3) 0.3027(2) 0.1808(5) 0.0669(13) Uani 1 1 d . . .
O3W O 0.2036(17) 0.6219(15) 0.624(4) 0.044(7) Uani 0.13 1 d PU . .
O4W O 0.2435(6) 0.6072(4) 0.4789(14) 0.080(3) Uani 0.50 1 d PU . .
O5W O 0.2858(10) 0.6217(10) 0.257(3) 0.058(5) Uani 0.20 1 d PU . .
O6W O 0.2500 0.7500 0.385(3) 0.106(6) Uani 0.50 2 d SPU . .
O7W O 0.2054(13) 0.7533(16) 0.452(3) 0.065(8) Uani 0.18 1 d P . .

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 0.0156(3) 0.0219(3) 0.0343(3) 0.0008(2) -0.00098(19) 0.00453(18)
Cu2 0.0202(4) 0.0202(4) 0.0343(4) 0.0065(3) -0.0043(3) 0.0000(3)
C1 0.0193(19) 0.0158(18) 0.0226(19) -0.0058(14) 0.0012(15) 0.0010(14)
C2 0.0181(18) 0.0169(17) 0.0233(18) -0.0007(15) 0.0007(15) -0.0016(15)
C3 0.0125(17) 0.0181(17) 0.0218(18) -0.0027(14) -0.0012(14) -0.0033(14)
C4 0.0173(18) 0.0173(17) 0.0174(17) -0.0023(14) -0.0023(14) -0.0009(14)
C5 0.024(2) 0.0153(17) 0.0124(17) -0.0022(13) 0.0005(14) -0.0049(14)
C6 0.0158(17) 0.0209(18) 0.0210(18) -0.0075(15) 0.0061(14) -0.0021(14)
C7 0.026(3) 0.015(2) 0.019(3) 0.000 0.000 -0.005(2)
C8 0.019(2) 0.0231(19) 0.033(2) -0.0046(17) 0.0026(16) 0.0032(16)
C9 0.0152(18) 0.020(2) 0.0257(19) -0.0003(15) 0.0004(15) -0.0039(15)
O1 0.0169(14) 0.0266(16) 0.060(2) -0.0041(15) -0.0037(14) 0.0031(13)
O2 0.0189(14) 0.0201(14) 0.055(2) 0.0045(13) 0.0010(14) 0.0061(12)
O3 0.0203(15) 0.0277(16) 0.062(2) 0.0193(15) 0.0101(15) 0.0033(12)
O4 0.0164(14) 0.0343(16) 0.0360(17) 0.0115(13) -0.0002(12) -0.0022(12)
O5 0.0230(14) 0.0192(14) 0.0340(16) 0.0060(12) -0.0019(12) -0.0010(11)
O6 0.053(3) 0.087(3) 0.054(3) -0.010(2) 0.002(2) 0.014(2)
O7 0.059(3) 0.034(2) 0.067(3) 0.0070(18) -0.004(2) -0.0098(18)
O1W 0.088(3) 0.034(2) 0.052(2) 0.0042(17) -0.004(2) -0.007(2)
O2W 0.085(3) 0.061(3) 0.055(3) -0.005(2) 0.001(2) -0.034(2)
O3W 0.056(14) 0.027(11) 0.050(14) 0.022(11) -0.014(12) -0.025(11)
O4W 0.087(7) 0.037(4) 0.115(8) -0.019(5) -0.077(6) 0.014(4)
O5W 0.032(9) 0.030(8) 0.112(15) 0.002(10) -0.029(10) 0.006(7)
O6W 0.111(13) 0.073(9) 0.134(14) 0.000 0.000 -0.007(10)
O7W 0.043(14) 0.09(2) 0.058(15) -0.038(15) 0.019(11) -0.005(13)

_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 O5 1.945(3) . ?
Cu1 O4 1.966(3) 4_465 ?
Cu1 O2 1.985(3) . ?
Cu1 O6 2.001(5) . ?
Cu1 O7 2.319(4) . ?
Cu2 O5 1.926(3) . ?
Cu2 O5 1.926(3) 5_566 ?
Cu2 O3 1.961(3) 4_465 ?
Cu2 O3 1.961(3) 8_656 ?
C1 C2 1.384(5) . ?
C1 C6 1.399(5) . ?
C1 C8 1.497(5) . ?
C2 C3 1.389(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(5) . ?
C3 C9 1.500(5) . ?
C4 C5 1.390(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.387(5) . ?
C5 C7 1.515(4) . ?
C6 H6 0.9300 . ?
C7 C5 1.515(4) 2 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O1 1.240(5) . ?
C8 O2 1.287(5) . ?
C9 O4 1.240(5) . ?
C9 O3 1.267(5) . ?
O3 Cu2 1.961(3) 4_565 ?
O4 Cu1 1.966(3) 4_565 ?
O5 H5 0.94(2) . ?
O6 H6A 0.95(2) . ?
O6 H6B 0.952(19) . ?
O7 H7C 0.92(2) . ?
O7 H7D 0.92(2) . ?
O3W O5W 1.10(4) 8_656 ?
O3W O4W 1.42(4) . ?
O5W O3W 1.10(4) 8_655 ?
O6W O7W 0.99(2) 2_565 ?
O6W O7W 0.99(2) . ?
O7W O7W 1.65(5) 2_565 ?

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
O5 Cu1 O4 88.16(12) . 4_465 ?
O5 Cu1 O2 90.87(13) . . ?
O4 Cu1 O2 167.61(13) 4_465 . ?
O5 Cu1 O6 176.05(16) . . ?
O4 Cu1 O6 88.15(16) 4_465 . ?
O2 Cu1 O6 92.45(16) . . ?
O5 Cu1 O7 96.12(14) . . ?
O4 Cu1 O7 97.74(15) 4_465 . ?
O2 Cu1 O7 94.65(14) . . ?
O6 Cu1 O7 85.74(19) . . ?
O5 Cu2 O5 180.0 . 5_566 ?
O5 Cu2 O3 92.72(12) . 4_465 ?
O5 Cu2 O3 87.28(12) 5_566 4_465 ?
O5 Cu2 O3 87.28(12) . 8_656 ?
O5 Cu2 O3 92.72(12) 5_566 8_656 ?
O3 Cu2 O3 180.000(1) 4_465 8_656 ?
C2 C1 C6 119.6(4) . . ?
C2 C1 C8 120.1(3) . . ?
C6 C1 C8 120.3(4) . . ?
C1 C2 C3 120.1(4) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 120.0(3) . . ?
C2 C3 C9 120.5(3) . . ?
C4 C3 C9 119.4(3) . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C6 C5 C4 119.2(3) . . ?
C6 C5 C7 121.2(3) . . ?
C4 C5 C7 119.6(3) . . ?
C5 C6 C1 120.7(3) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C5 C7 C5 113.1(4) 2 . ?
C5 C7 H7A 109.0 2 . ?
C5 C7 H7A 109.0 . . ?
C5 C7 H7B 109.0 2 . ?
C5 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
O1 C8 O2 122.5(4) . . ?
O1 C8 C1 120.9(4) . . ?
O2 C8 C1 116.6(3) . . ?
O4 C9 O3 125.8(4) . . ?
O4 C9 C3 117.7(3) . . ?
O3 C9 C3 116.5(3) . . ?
C8 O2 Cu1 107.8(3) . . ?
C9 O3 Cu2 131.6(3) . 4_565 ?
C9 O4 Cu1 123.3(3) . 4_565 ?
Cu2 O5 Cu1 107.79(14) . . ?
Cu2 O5 H5 127(5) . . ?
Cu1 O5 H5 114(5) . . ?
Cu1 O6 H6A 122(5) . . ?
Cu1 O6 H6B 102.2(17) . . ?
H6A O6 H6B 105(3) . . ?
Cu1 O7 H7C 112(4) . . ?
Cu1 O7 H7D 119(4) . . ?
H7C O7 H7D 109(3) . . ?
O5W O3W O4W 137(3) 8_656 . ?
O7W O6W O7W 114(4) 2_565 . ?
O6W O7W O7W 33(2) . 2_565 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 O1W 0.94(2) 1.83(3) 2.724(5) 159(7) 7_576
O6 H6A O2W 0.95(2) 2.32(3) 3.235(7) 162(7) 5_565
O7 H7C O1W 0.92(2) 1.83(2) 2.743(6) 168(7) .
O7 H7D O7W 0.92(2) 1.91(4) 2.78(3) 156(7) .
O7 H7D O6W 0.92(2) 2.29(6) 2.986(13) 132(6) .

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.07
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.401
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.123