# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Catalina Ruiz-Perez'
_publ_contact_author_email       CARUIZ@ULL.ES

_publ_section_title              
;
Well-resolved unusual alternating cyclic water
tetramers embedded in a crystal host
;
loop_
_publ_author_name
'Catalina Ruiz-Perez'
'Laura Canadillas-Delgado'
'Fernando S. Delgado'
'Oscar Fabelo'
;
M.Julve
;
'Ana Labrador'
'F Lloret'
'Jorge Pasan'

# Attachment 'Compound-1.cif'

data_test
_database_code_depnum_ccdc_archive 'CCDC 692490'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H26 Co2 O20'
_chemical_formula_weight         584.17

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'
Co Co 0.3494 0.9721 '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_int_tables_number      2

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

_cell_length_a                   10.847(2)
_cell_length_b                   11.107(2)
_cell_length_c                   11.483(2)
_cell_angle_alpha                82.93(3)
_cell_angle_beta                 63.02(3)
_cell_angle_gamma                62.12(3)
_cell_volume                     1082.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_exptl_absorpt_coefficient_mu    1.626
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72930
_diffrn_source                   synchrotron
_diffrn_source_type              'ESRF-CRG BM16'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9.6
_diffrn_radiation_detector       'ADSC Q210r CCD (binned mode)'
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_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            34999
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         29.10
_reflns_number_total             4903
_reflns_number_gt                4632
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MxCube (ESRF, 2006)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_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 F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0688P)²+0.2158P] where P=(Fo²+2Fc²)/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         4903
_refine_ls_number_parameters     399
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0987
_refine_ls_wR_factor_gt          0.0965
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C5 C 0.23695(11) 0.79757(11) 0.07461(11) 0.0110(2) Uani 1 1 d . . .
C2 C 0.10942(12) 0.90291(11) 0.04101(11) 0.0108(2) Uani 1 1 d . . .
C1 C -0.00351(12) 1.02975(11) 0.11726(11) 0.0112(2) Uani 1 1 d . . .
C4 C -0.01793(12) 1.06993(11) 0.24429(11) 0.0119(2) Uani 1 1 d . . .
C3 C 0.11089(12) 0.87540(10) -0.07475(11) 0.0117(2) Uani 1 1 d . . .
C10 C 0.26531(11) 0.20263(11) -0.07593(11) 0.0108(2) Uani 1 1 d . . .
C7 C 0.39192(12) 0.09733(10) -0.04157(11) 0.0106(2) Uani 1 1 d . . .
C8 C 0.39640(12) 0.12807(10) 0.07006(11) 0.0117(2) Uani 1 1 d . . .
C6 C 0.49708(12) -0.03280(11) -0.11318(11) 0.0110(2) Uani 1 1 d . . .
C9 C 0.50375(11) -0.07429(11) -0.23652(11) 0.0112(2) Uani 1 1 d . . .
Co2 Co 0.5000 0.5000 0.0000 0.00994(9) Uani 1 2 d S . .
Co3 Co 0.5000 0.0000 -0.5000 0.01047(9) Uani 1 2 d S . .
Co1 Co 0.0000 1.0000 0.5000 0.01035(9) Uani 1 2 d S . .
Co4 Co 0.0000 0.5000 0.0000 0.01014(9) Uani 1 2 d S . .
O7 O 0.21762(9) 0.32744(8) -0.04195(8) 0.01309(17) Uani 1 1 d . . .
O5 O 0.53757(9) -0.00691(8) -0.33442(8) 0.01284(17) Uani 1 1 d . . .
O3 O 0.28853(9) 0.67341(8) 0.03394(8) 0.01298(17) Uani 1 1 d . . .
O1 O -0.04462(9) 0.99722(8) 0.33852(8) 0.01271(17) Uani 1 1 d . . .
O8 O 0.21109(9) 0.16189(8) -0.12882(8) 0.01372(17) Uani 1 1 d . . .
O6 O 0.48164(10) -0.17545(8) -0.23778(8) 0.01579(17) Uani 1 1 d . . .
O4 O 0.28735(9) 0.83574(8) 0.13287(8) 0.01416(17) Uani 1 1 d . . .
O2 O -0.00867(10) 1.17729(8) 0.25178(9) 0.01788(18) Uani 1 1 d . . .
O7W O 0.08187(10) 0.56603(8) -0.18667(8) 0.01634(17) Uani 1 1 d . . .
O8W O 0.05441(10) 0.61340(8) 0.08105(9) 0.01544(17) Uani 1 1 d . . .
O5W O 0.51205(10) 0.18017(8) -0.52926(8) 0.01865(18) Uani 1 1 d . . .
O6W O 0.25497(9) 0.09793(8) -0.36859(8) 0.01492(17) Uani 1 1 d . . .
O4W O 0.45267(9) 0.39370(8) -0.09792(9) 0.01471(17) Uani 1 1 d . . .
O3W O 0.39260(9) 0.43550(8) 0.18328(8) 0.01506(17) Uani 1 1 d . . .
O2W O 0.22956(9) 0.94575(9) 0.36328(9) 0.01994(19) Uani 1 1 d . . .
O1W O 0.06485(9) 0.79048(8) 0.50568(8) 0.01636(17) Uani 1 1 d . . .
O9W O 0.37141(9) 0.42768(8) 0.61390(8) 0.02045(18) Uani 1 1 d . . .
O10W O 0.36794(10) 0.57100(9) 0.39832(9) 0.02232(19) Uani 1 1 d . . .
O11W O 0.10144(9) 0.45224(8) 0.30109(8) 0.02022(18) Uani 1 1 d . . .
O12W O -0.10166(10) 0.68369(8) 0.47964(9) 0.02192(18) Uani 1 1 d . . .
H42W H 0.369(2) 0.3784(19) -0.0689(18) 0.025(4) Uiso 1 1 d . . .
H41W H 0.531(3) 0.315(3) -0.115(2) 0.047(6) Uiso 1 1 d . . .
H32W H 0.297(2) 0.4541(19) 0.2138(18) 0.038(5) Uiso 1 1 d . . .
H31W H 0.454(3) 0.342(3) 0.185(3) 0.057(7) Uiso 1 1 d . . .
H12W H 0.008(2) 0.7637(19) 0.4965(18) 0.026(4) Uiso 1 1 d . . .
H11W H 0.032(3) 0.793(2) 0.595(2) 0.052(6) Uiso 1 1 d . . .
H21W H 0.297(2) 0.9631(19) 0.3617(18) 0.030(5) Uiso 1 1 d . . .
H22W H 0.256(3) 0.911(2) 0.287(2) 0.045(6) Uiso 1 1 d . . .
H62W H 0.201(2) 0.054(2) -0.360(2) 0.035(5) Uiso 1 1 d . . .
H61W H 0.243(2) 0.116(2) -0.291(2) 0.035(5) Uiso 1 1 d . . .
H51W H 0.464(2) 0.250(2) -0.4781(18) 0.024(4) Uiso 1 1 d . . .
H52W H 0.510(2) 0.2003(19) -0.603(2) 0.031(4) Uiso 1 1 d . . .
H82W H 0.137(2) 0.624(2) 0.0549(19) 0.028(4) Uiso 1 1 d . . .
H81W H -0.020(3) 0.689(2) 0.099(2) 0.042(6) Uiso 1 1 d . . .
H72W H 0.183(2) 0.519(2) -0.2423(19) 0.040(5) Uiso 1 1 d . . .
H71W H 0.055(3) 0.657(3) -0.191(3) 0.055(7) Uiso 1 1 d . . .
H2 H 0.3241(19) 0.2166(17) 0.1207(16) 0.016(4) Uiso 1 1 d . . .
H1 H 0.1883(19) 0.7887(17) -0.1276(16) 0.016(4) Uiso 1 1 d . . .
H9A H 0.365(2) 0.474(2) 0.549(2) 0.044(5) Uiso 1 1 d . . .
H9B H 0.457(2) 0.417(2) 0.6195(19) 0.043(5) Uiso 1 1 d . . .
H10A H 0.392(3) 0.532(2) 0.326(2) 0.054(6) Uiso 1 1 d . . .
H10B H 0.281(3) 0.647(2) 0.419(2) 0.058(6) Uiso 1 1 d . . .
H12A H -0.031(3) 0.615(2) 0.411(2) 0.049(6) Uiso 1 1 d . . .
H12B H -0.164(2) 0.743(2) 0.4532(18) 0.042(5) Uiso 1 1 d . . .
H11A H 0.051(3) 0.450(2) 0.260(2) 0.061(6) Uiso 1 1 d . . .
H11B H 0.112(2) 0.389(2) 0.358(2) 0.055(6) Uiso 1 1 d . . .


_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
C5 O4 1.2429(15) . ?
C5 O3 1.2778(14) . ?
C5 C2 1.5135(15) . ?
C2 C3 1.3917(17) . ?
C2 C1 1.4029(17) . ?
C1 C3 1.3951(15) 2_575 ?
C1 C4 1.4964(16) . ?
C4 O2 1.2588(14) . ?
C4 O1 1.2752(14) . ?
C3 C1 1.3951(15) 2_575 ?
C10 O8 1.2490(15) . ?
C10 O7 1.2732(14) . ?
C10 C7 1.5117(15) . ?
C7 C8 1.3935(17) . ?
C7 C6 1.4021(17) . ?
C8 C6 1.3951(15) 2_655 ?
C6 C8 1.3951(15) 2_655 ?
C6 C9 1.5034(16) . ?
C9 O6 1.2567(14) . ?
C9 O5 1.2781(14) . ?
Co2 O4W 2.0832(10) . ?
Co2 O4W 2.0832(10) 2_665 ?
Co2 O3 2.0892(13) 2_665 ?
Co2 O3 2.0892(13) . ?
Co2 O3W 2.1175(11) . ?
Co2 O3W 2.1175(11) 2_665 ?
Co3 O5W 2.0430(9) 2_654 ?
Co3 O5W 2.0430(9) . ?
Co3 O5 2.1035(9) . ?
Co3 O5 2.1035(9) 2_654 ?
Co3 O6W 2.1412(14) 2_654 ?
Co3 O6W 2.1412(14) . ?
Co1 O2W 2.0761(13) 2_576 ?
Co1 O2W 2.0761(13) . ?
Co1 O1W 2.0948(9) . ?
Co1 O1W 2.0948(9) 2_576 ?
Co1 O1 2.1251(9) 2_576 ?
Co1 O1 2.1251(9) . ?
Co4 O8W 2.0696(10) . ?
Co4 O8W 2.0696(10) 2_565 ?
Co4 O7W 2.1014(11) 2_565 ?
Co4 O7W 2.1014(11) . ?
Co4 O7 2.1075(13) 2_565 ?
Co4 O7 2.1075(13) . ?

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
O4 C5 O3 125.26(10) . . ?
O4 C5 C2 119.73(10) . . ?
O3 C5 C2 114.95(10) . . ?
C3 C2 C1 119.00(10) . . ?
C3 C2 C5 118.16(10) . . ?
C1 C2 C5 122.72(11) . . ?
C3 C1 C2 119.05(11) 2_575 . ?
C3 C1 C4 117.18(10) 2_575 . ?
C2 C1 C4 123.77(10) . . ?
O2 C4 O1 124.54(11) . . ?
O2 C4 C1 116.99(10) . . ?
O1 C4 C1 118.40(10) . . ?
C2 C3 C1 121.95(11) . 2_575 ?
O8 C10 O7 125.29(10) . . ?
O8 C10 C7 118.65(10) . . ?
O7 C10 C7 115.97(10) . . ?
C8 C7 C6 119.43(10) . . ?
C8 C7 C10 118.50(10) . . ?
C6 C7 C10 121.91(11) . . ?
C7 C8 C6 121.87(11) . 2_655 ?
C8 C6 C7 118.69(11) 2_655 . ?
C8 C6 C9 118.00(10) 2_655 . ?
C7 C6 C9 123.29(10) . . ?
O6 C9 O5 124.74(11) . . ?
O6 C9 C6 117.93(10) . . ?
O5 C9 C6 117.28(10) . . ?
O4W Co2 O4W 180.00(5) . 2_665 ?
O4W Co2 O3 90.33(4) . 2_665 ?
O4W Co2 O3 89.67(4) 2_665 2_665 ?
O4W Co2 O3 89.67(4) . . ?
O4W Co2 O3 90.33(4) 2_665 . ?
O3 Co2 O3 180.00(5) 2_665 . ?
O4W Co2 O3W 92.73(4) . . ?
O4W Co2 O3W 87.27(4) 2_665 . ?
O3 Co2 O3W 88.70(5) 2_665 . ?
O3 Co2 O3W 91.30(5) . . ?
O4W Co2 O3W 87.27(4) . 2_665 ?
O4W Co2 O3W 92.73(4) 2_665 2_665 ?
O3 Co2 O3W 91.30(5) 2_665 2_665 ?
O3 Co2 O3W 88.70(5) . 2_665 ?
O3W Co2 O3W 180.00(4) . 2_665 ?
O5W Co3 O5W 180.0 2_654 . ?
O5W Co3 O5 92.13(4) 2_654 . ?
O5W Co3 O5 87.87(4) . . ?
O5W Co3 O5 87.87(4) 2_654 2_654 ?
O5W Co3 O5 92.13(4) . 2_654 ?
O5 Co3 O5 180.000(1) . 2_654 ?
O5W Co3 O6W 93.63(5) 2_654 2_654 ?
O5W Co3 O6W 86.37(5) . 2_654 ?
O5 Co3 O6W 92.95(4) . 2_654 ?
O5 Co3 O6W 87.05(4) 2_654 2_654 ?
O5W Co3 O6W 86.37(5) 2_654 . ?
O5W Co3 O6W 93.63(5) . . ?
O5 Co3 O6W 87.05(4) . . ?
O5 Co3 O6W 92.95(4) 2_654 . ?
O6W Co3 O6W 180.0 2_654 . ?
O2W Co1 O2W 180.000(1) 2_576 . ?
O2W Co1 O1W 92.12(6) 2_576 . ?
O2W Co1 O1W 87.88(6) . . ?
O2W Co1 O1W 87.88(6) 2_576 2_576 ?
O2W Co1 O1W 92.12(6) . 2_576 ?
O1W Co1 O1W 180.000(1) . 2_576 ?
O2W Co1 O1 87.17(4) 2_576 2_576 ?
O2W Co1 O1 92.83(4) . 2_576 ?
O1W Co1 O1 90.67(4) . 2_576 ?
O1W Co1 O1 89.33(4) 2_576 2_576 ?
O2W Co1 O1 92.83(4) 2_576 . ?
O2W Co1 O1 87.17(4) . . ?
O1W Co1 O1 89.33(4) . . ?
O1W Co1 O1 90.67(4) 2_576 . ?
O1 Co1 O1 180.000(1) 2_576 . ?
O8W Co4 O8W 180.00(4) . 2_565 ?
O8W Co4 O7W 86.46(4) . 2_565 ?
O8W Co4 O7W 93.54(4) 2_565 2_565 ?
O8W Co4 O7W 93.54(4) . . ?
O8W Co4 O7W 86.46(4) 2_565 . ?
O7W Co4 O7W 180.00(5) 2_565 . ?
O8W Co4 O7 89.55(4) . 2_565 ?
O8W Co4 O7 90.45(4) 2_565 2_565 ?
O7W Co4 O7 93.77(5) 2_565 2_565 ?
O7W Co4 O7 86.23(5) . 2_565 ?
O8W Co4 O7 90.45(4) . . ?
O8W Co4 O7 89.55(4) 2_565 . ?
O7W Co4 O7 86.23(5) 2_565 . ?
O7W Co4 O7 93.77(5) . . ?
O7 Co4 O7 180.0 2_565 . ?
C10 O7 Co4 129.74(7) . . ?
C9 O5 Co3 127.09(8) . . ?
C5 O3 Co2 130.40(7) . . ?
C4 O1 Co1 122.80(8) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        29.10
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.547
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.082


