# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global

_journal_coden_Cambridge         182
_journal_volume                  ?
_journal_year                    ?
_journal_page_first              ?

_publ_requested_journal          'Chemical Communications'

loop_
_publ_author_name
'Baoqing Ma'
'Song Gao'
'Hao-Ling Sun'

_publ_contact_author_name        'Baoqing Ma'
_publ_contact_author_address     
;
Chemistry
Peking University
Beijing
Beijing
100871
CHINA
;

_publ_contact_author_email       MABQING@YAHOO.COM

_publ_section_title              
;
Observation of an octameric water cluster containing
book-shaped hexamer in a 4f-3d complex
;

data_c2c
_database_code_depnum_ccdc_archive 'CCDC 261999'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H32 Co N10 O12 Y'
_chemical_formula_weight         824.46

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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   19.384(4)
_cell_length_b                   8.2478(16)
_cell_length_c                   22.090(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.02(3)
_cell_angle_gamma                90.00
_cell_volume                     3477.9(12)
_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       prismatic
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1680
_exptl_absorpt_coefficient_mu    2.210
_exptl_absorpt_correction_type   SORTAV
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean 0.71
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21940
_diffrn_reflns_av_R_equivalents  0.1748
_diffrn_reflns_av_sigmaI/netI    0.1276
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.75
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3057
_reflns_number_gt                1862
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius Kappa CCD'
_computing_cell_refinement       'Denzo Scalepack'
_computing_data_reduction        'Denzo Maxus'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Siemens SHELXTL (1990)'
_computing_publication_material  'Siemnes SHELXL-97'

_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^)+(0.0278P)^2^+1.2726P] 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         3057
_refine_ls_number_parameters     260
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0542
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_restrained_S_all      0.987
_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
Y1 Y 0.5000 0.63741(8) 0.2500 0.0253(2) Uani 1 2 d S . .
Co1 Co 0.7500 0.7500 0.5000 0.0265(3) Uani 1 2 d S . .
O1 O 0.60805(15) 0.7457(4) 0.24654(12) 0.0295(8) Uani 1 1 d . . .
O2 O 0.52968(15) 0.5354(4) 0.15995(13) 0.0305(8) Uani 1 1 d . . .
O3 O 0.57604(17) 0.4098(4) 0.27396(16) 0.0355(9) Uani 1 1 d D . .
O4 O 0.51847(17) 0.8645(4) 0.31679(14) 0.0336(8) Uani 1 1 d D . .
O5 O 0.59062(18) 0.2390(5) 0.37842(15) 0.0451(10) Uani 1 1 d D . .
O6 O 0.4465(2) 1.1672(4) 0.32653(15) 0.0429(10) Uani 1 1 d D . .
N1 N 0.6630(2) 0.6651(5) 0.23396(16) 0.0289(10) Uani 1 1 d . . .
N2 N 0.54833(19) 0.6313(5) 0.11681(16) 0.0282(10) Uani 1 1 d . . .
N3 N 0.6390(2) 0.9120(5) 0.40508(17) 0.0370(12) Uani 1 1 d . . .
N4 N 0.6844(3) 0.4329(6) 0.4523(2) 0.0741(17) Uani 1 1 d . . .
N5 N 0.8507(2) 0.7249(6) 0.40881(19) 0.0596(15) Uani 1 1 d . . .
C1 C 0.7136(3) 0.6217(6) 0.2813(2) 0.0376(13) Uani 1 1 d . . .
H1A H 0.7070 0.6382 0.3216 0.045 Uiso 1 1 calc R . .
C2 C 0.7744(3) 0.5536(6) 0.2701(3) 0.0440(15) Uani 1 1 d . . .
H2A H 0.8094 0.5245 0.3026 0.053 Uiso 1 1 calc R . .
C3 C 0.7835(3) 0.5284(6) 0.2105(2) 0.0466(15) Uani 1 1 d . . .
H3A H 0.8251 0.4839 0.2025 0.056 Uiso 1 1 calc R . .
C4 C 0.7309(3) 0.5694(6) 0.1630(2) 0.0386(14) Uani 1 1 d . . .
H4C H 0.7367 0.5513 0.1226 0.046 Uiso 1 1 calc R . .
C5 C 0.6699(2) 0.6367(6) 0.1745(2) 0.0306(12) Uani 1 1 d . . .
C6 C 0.6146(3) 0.6906(6) 0.1232(2) 0.0290(13) Uani 1 1 d . . .
C7 C 0.6314(3) 0.7910(6) 0.0779(2) 0.0405(14) Uani 1 1 d . . .
H7A H 0.6765 0.8327 0.0815 0.049 Uiso 1 1 calc R . .
C8 C 0.5817(3) 0.8300(7) 0.0275(2) 0.0515(16) Uani 1 1 d . . .
H8A H 0.5927 0.9000 -0.0025 0.062 Uiso 1 1 calc R . .
C9 C 0.5164(3) 0.7646(7) 0.0219(2) 0.0478(16) Uani 1 1 d . . .
H9A H 0.4826 0.7881 -0.0123 0.057 Uiso 1 1 calc R . .
C10 C 0.5007(3) 0.6642(6) 0.0670(2) 0.0384(14) Uani 1 1 d . . .
H10A H 0.4564 0.6182 0.0628 0.046 Uiso 1 1 calc R . .
C11 C 0.6817(2) 0.8532(6) 0.4408(2) 0.0259(11) Uani 1 1 d . . .
C12 C 0.7099(3) 0.5493(7) 0.4713(2) 0.0407(14) Uani 1 1 d . . .
C13 C 0.8131(3) 0.7360(6) 0.4427(2) 0.0356(13) Uani 1 1 d . . .
H6 H 0.610(2) 0.135(3) 0.3822(17) 0.032(14) Uiso 1 1 d D . .
H5 H 0.617(2) 0.303(4) 0.4099(17) 0.08(2) Uiso 1 1 d D . .
H8 H 0.4898(14) 1.209(7) 0.347(2) 0.10(2) Uiso 1 1 d D . .
H7 H 0.4137(18) 1.184(7) 0.3527(19) 0.09(2) Uiso 1 1 d D . .
H2 H 0.578(3) 0.338(5) 0.2416(15) 0.11(3) Uiso 1 1 d D . .
H4 H 0.5581(18) 0.877(6) 0.348(2) 0.10(2) Uiso 1 1 d D . .
H3 H 0.489(2) 0.953(5) 0.321(2) 0.08(2) Uiso 1 1 d D . .
H1 H 0.573(3) 0.347(5) 0.3094(13) 0.08(2) 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
Y1 0.0235(4) 0.0290(4) 0.0233(4) 0.000 0.0037(3) 0.000
Co1 0.0237(6) 0.0308(6) 0.0239(5) 0.0004(5) 0.0011(4) 0.0010(5)
O1 0.0177(18) 0.035(2) 0.0360(19) -0.0053(16) 0.0051(14) 0.0029(17)
O2 0.038(2) 0.030(2) 0.0260(18) 0.0035(16) 0.0124(16) -0.0088(17)
O3 0.042(2) 0.034(2) 0.032(2) 0.0075(19) 0.0109(18) 0.0070(18)
O4 0.032(2) 0.035(2) 0.032(2) -0.0100(17) -0.0017(17) 0.003(2)
O5 0.054(3) 0.036(2) 0.040(2) 0.005(2) -0.0084(18) 0.004(2)
O6 0.035(2) 0.043(3) 0.053(2) -0.0148(19) 0.015(2) -0.003(2)
N1 0.023(2) 0.033(3) 0.031(2) 0.002(2) 0.004(2) 0.000(2)
N2 0.028(3) 0.033(3) 0.023(2) -0.004(2) 0.0026(19) 0.002(2)
N3 0.033(3) 0.041(3) 0.034(2) 0.011(2) -0.004(2) 0.007(2)
N4 0.087(4) 0.049(4) 0.079(4) -0.010(3) -0.006(3) -0.023(3)
N5 0.052(3) 0.090(4) 0.041(3) 0.008(3) 0.019(3) 0.015(3)
C1 0.034(3) 0.046(4) 0.030(3) -0.002(3) -0.001(3) 0.001(3)
C2 0.030(3) 0.042(4) 0.057(4) 0.001(3) 0.000(3) 0.007(3)
C3 0.035(3) 0.051(4) 0.057(4) 0.000(3) 0.015(3) 0.015(3)
C4 0.033(3) 0.048(4) 0.038(3) -0.004(3) 0.014(3) 0.006(3)
C5 0.027(3) 0.030(3) 0.037(3) 0.000(3) 0.010(2) -0.004(3)
C6 0.026(3) 0.036(3) 0.024(3) -0.004(2) 0.003(2) 0.000(3)
C7 0.037(3) 0.048(4) 0.040(3) 0.000(3) 0.016(3) -0.010(3)
C8 0.070(5) 0.058(4) 0.029(3) 0.008(3) 0.012(3) 0.001(4)
C9 0.048(4) 0.066(4) 0.026(3) 0.007(3) -0.003(3) 0.006(3)
C10 0.034(3) 0.054(4) 0.025(3) 0.001(3) 0.000(3) 0.005(3)
C11 0.026(3) 0.027(3) 0.025(3) 0.000(2) 0.006(2) -0.006(3)
C12 0.040(4) 0.042(4) 0.037(3) -0.009(3) -0.002(3) 0.001(3)
C13 0.033(3) 0.041(4) 0.031(3) 0.001(3) -0.002(3) 0.005(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
Y1 O1 2.291(3) . ?
Y1 O1 2.291(3) 2_655 ?
Y1 O2 2.323(3) . ?
Y1 O2 2.323(3) 2_655 ?
Y1 O4 2.373(3) . ?
Y1 O4 2.373(3) 2_655 ?
Y1 O3 2.389(3) 2_655 ?
Y1 O3 2.389(3) . ?
Co1 C12 1.891(6) . ?
Co1 C12 1.891(6) 7_666 ?
Co1 C11 1.893(5) 7_666 ?
Co1 C11 1.893(5) . ?
Co1 C13 1.912(6) 7_666 ?
Co1 C13 1.912(6) . ?
O1 N1 1.326(4) . ?
O2 N2 1.336(4) . ?
N1 C1 1.351(5) . ?
N1 C5 1.364(5) . ?
N2 C10 1.335(5) . ?
N2 C6 1.358(5) . ?
N3 C11 1.147(5) . ?
N4 C12 1.127(6) . ?
N5 C13 1.134(6) . ?
C1 C2 1.367(6) . ?
C2 C3 1.374(6) . ?
C3 C4 1.374(6) . ?
C4 C5 1.369(6) . ?
C5 C6 1.486(6) . ?
C6 C7 1.380(6) . ?
C7 C8 1.377(6) . ?
C8 C9 1.363(7) . ?
C9 C10 1.368(7) . ?

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 Y1 O1 134.10(16) . 2_655 ?
O1 Y1 O2 75.43(10) . . ?
O1 Y1 O2 122.28(10) 2_655 . ?
O1 Y1 O2 122.28(10) . 2_655 ?
O1 Y1 O2 75.43(10) 2_655 2_655 ?
O2 Y1 O2 137.52(16) . 2_655 ?
O1 Y1 O4 70.91(11) . . ?
O1 Y1 O4 73.22(11) 2_655 . ?
O2 Y1 O4 141.77(12) . . ?
O2 Y1 O4 77.67(11) 2_655 . ?
O1 Y1 O4 73.22(11) . 2_655 ?
O1 Y1 O4 70.91(11) 2_655 2_655 ?
O2 Y1 O4 77.67(11) . 2_655 ?
O2 Y1 O4 141.77(12) 2_655 2_655 ?
O4 Y1 O4 75.73(16) . 2_655 ?
O1 Y1 O3 146.27(12) . 2_655 ?
O1 Y1 O3 77.36(11) 2_655 2_655 ?
O2 Y1 O3 76.16(11) . 2_655 ?
O2 Y1 O3 70.71(11) 2_655 2_655 ?
O4 Y1 O3 141.15(12) . 2_655 ?
O4 Y1 O3 117.53(12) 2_655 2_655 ?
O1 Y1 O3 77.36(11) . . ?
O1 Y1 O3 146.27(12) 2_655 . ?
O2 Y1 O3 70.71(11) . . ?
O2 Y1 O3 76.16(11) 2_655 . ?
O4 Y1 O3 117.53(12) . . ?
O4 Y1 O3 141.15(12) 2_655 . ?
O3 Y1 O3 76.38(16) 2_655 . ?
C12 Co1 C12 180.000(1) . 7_666 ?
C12 Co1 C11 92.0(2) . 7_666 ?
C12 Co1 C11 88.0(2) 7_666 7_666 ?
C12 Co1 C11 88.0(2) . . ?
C12 Co1 C11 92.0(2) 7_666 . ?
C11 Co1 C11 180.000(1) 7_666 . ?
C12 Co1 C13 90.1(2) . 7_666 ?
C12 Co1 C13 89.9(2) 7_666 7_666 ?
C11 Co1 C13 91.22(19) 7_666 7_666 ?
C11 Co1 C13 88.78(19) . 7_666 ?
C12 Co1 C13 89.9(2) . . ?
C12 Co1 C13 90.1(2) 7_666 . ?
C11 Co1 C13 88.78(19) 7_666 . ?
C11 Co1 C13 91.22(19) . . ?
C13 Co1 C13 180.000(1) 7_666 . ?
N1 O1 Y1 125.7(3) . . ?
N2 O2 Y1 122.3(2) . . ?
O1 N1 C1 118.1(4) . . ?
O1 N1 C5 120.3(4) . . ?
C1 N1 C5 121.4(4) . . ?
O2 N2 C10 118.3(4) . . ?
O2 N2 C6 120.5(3) . . ?
C10 N2 C6 121.1(4) . . ?
N1 C1 C2 120.0(5) . . ?
C1 C2 C3 119.7(5) . . ?
C2 C3 C4 119.5(5) . . ?
C5 C4 C3 120.6(5) . . ?
N1 C5 C4 118.7(4) . . ?
N1 C5 C6 120.3(4) . . ?
C4 C5 C6 120.8(4) . . ?
N2 C6 C7 118.6(4) . . ?
N2 C6 C5 121.0(4) . . ?
C7 C6 C5 120.1(4) . . ?
C8 C7 C6 120.4(5) . . ?
C9 C8 C7 119.2(5) . . ?
C8 C9 C10 119.6(5) . . ?
N2 C10 C9 120.9(5) . . ?
N3 C11 Co1 178.0(4) . . ?
N4 C12 Co1 177.2(5) . . ?
N5 C13 Co1 178.8(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.094