# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_H2O@C60_20K
#TrackingRef '18722_web_deposit_cif_file_0_ShinobuAoyagi_1363834453.H2O@C60_20K.cif'


_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H2 O'
_chemical_formula_weight         738.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0003 0.0007 'S. Sasaki (1989) KEK Report 88-14.'
O O 0.0010 0.0028 'S. Sasaki (1989) KEK Report 88-14.'
H H 0.0000 0.0000 'S. Sasaki (1989) KEK Report 88-14.'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'P a -3'

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

_cell_length_a                   14.06690(10)
_cell_length_b                   14.06690(10)
_cell_length_c                   14.06690(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2783.53(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    20
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      20
_diffrn_radiation_wavelength     0.49917
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'SPring-8 BL02B1 bending magnet'
_diffrn_radiation_monochromator  'Si 311'
_diffrn_measurement_device_type  'Large cylindrical imaging plate camera'
_diffrn_measurement_method       'Oscilation method'
_diffrn_detector_area_resol_mean 10
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13430
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.088
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         48.99
_reflns_number_total             13430
_reflns_number_gt                8831
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku Corporation)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against reflections with F^2^ > 1.0sigma(F^2^).
The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F. 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^)+(0.1000P)^2^+0.0000P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7591
_refine_ls_number_parameters     127
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0901
_refine_ls_wR_factor_gt          0.0851
_refine_ls_goodness_of_fit_ref   ?
_refine_ls_restrained_S_all      0.472
_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
O1 O 0.0000 0.0000 0.0000 0.01827(6) Uiso 1 6 d SG . .
H11 H 0.0606 0.0305 0.0063 0.022 Uiso 0.167 1 d PG . .
H12 H -0.0402 0.0472 -0.0281 0.022 Uiso 0.167 1 d PG . .
C1A C 0.228875(11) -0.033247(12) 0.101859(12) 0.00708(2) Uani 0.7925(4) 1 d PD
. .
C2A C 0.246372(11) -0.055032(11) 0.006736(12) 0.00720(2) Uani 0.7925(4) 1 d PD
. .
C3A C 0.20744(6) 0.06409(5) 0.12963(7) 0.00686(3) Uani 0.7925(4) 1 d PD . .
C4A C 0.206331(11) -0.140764(11) -0.034964(11) 0.00714(2) Uani 0.7925(4) 1 d PD
. .
C5A C 0.170582(11) -0.096536(11) 0.159467(12) 0.00716(2) Uani 0.7925(4) 1 d PD
. .
C6A C 0.222704(16) 0.113059(13) -0.038288(16) 0.00708(2) Uani 0.7925(4) 1 d PD
. .
C7A C 0.243260(11) 0.019579(12) -0.064761(11) 0.00714(2) Uani 0.7925(4) 1 d PD
. .
C8A C 0.20430(4) 0.13626(7) 0.06066(4) 0.00709(4) Uani 0.7925(4) 1 d PD . .
C9A C 0.150436(11) -0.201250(11) 0.020108(12) 0.00711(2) Uani 0.7925(4) 1 d PD
. .
C10A C 0.132234(11) -0.178707(11) 0.119402(12) 0.00715(2) Uani 0.7925(4) 1 d PD
. .
C1B C 0.10142(6) -0.03329(7) 0.22859(8) 0.00809(4) Uiso 0.2075(4) 1 d PD . .
C2B C 0.13162(4) -0.11540(4) 0.18201(4) 0.00809(4) Uiso 0.2075(4) 1 d PD . .
C3B C 0.1369(3) 0.05958(17) 0.1999(2) 0.00809(4) Uiso 0.2075(4) 1 d PD . .
C4B C 0.06273(4) -0.18797(5) 0.15620(5) 0.00809(4) Uiso 0.2075(4) 1 d PD . .
C5B C 0.00136(4) -0.02019(4) 0.25203(4) 0.00809(4) Uiso 0.2075(4) 1 d PD . .
C6B C 0.23875(5) -0.02113(4) 0.07921(5) 0.00809(4) Uiso 0.2075(4) 1 d PD . .
C7B C 0.20150(4) -0.10914(4) 0.10610(4) 0.00809(4) Uiso 0.2075(4) 1 d PD . .
C8B C 0.2058(3) 0.0639(2) 0.1276(3) 0.00809(4) Uiso 0.2075(4) 1 d PD . .
C9B C -0.03316(4) -0.17546(4) 0.17795(5) 0.00809(4) Uiso 0.2075(4) 1 d PD . .
C10B C -0.06461(4) -0.08979(4) 0.22678(4) 0.00809(4) Uiso 0.2075(4) 1 d PD . .

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
C1A 0.00575(4) 0.00800(4) 0.00749(4) -0.00010(3) -0.00103(3) 0.00038(3)
C2A 0.00544(4) 0.00803(4) 0.00814(4) -0.00020(3) -0.00026(3) 0.00055(3)
C3A 0.00576(6) 0.00774(4) 0.00710(7) -0.00024(4) -0.00146(5) -0.00053(3)
C4A 0.00620(4) 0.00705(4) 0.00816(5) -0.00019(3) 0.00018(3) 0.00129(3)
C5A 0.00696(4) 0.00746(4) 0.00706(4) 0.00051(3) -0.00109(3) 0.00066(3)
C6A 0.00583(5) 0.00700(5) 0.00841(5) 0.00024(4) 0.00062(3) -0.00142(4)
C7A 0.00562(4) 0.00803(4) 0.00778(4) 0.00001(3) 0.00070(3) -0.00025(3)
C8A 0.00548(8) 0.00773(5) 0.00807(5) -0.00072(4) -0.00055(5) -0.00182(7)
C9A 0.00690(4) 0.00638(4) 0.00806(4) 0.00001(3) -0.00019(3) 0.00140(3)
C10A 0.00739(4) 0.00655(4) 0.00750(4) 0.00074(3) -0.00072(3) 0.00095(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
C1A C2A 1.3946(2) . ?
C1A C3A 1.4555(5) . ?
C1A C5A 1.4566(2) . ?
C2A C7A 1.4543(2) . ?
C2A C4A 1.4546(2) . ?
C3A C8A 1.4049(11) . ?
C3A C8A 1.4520(5) 5 ?
C4A C9A 1.3937(2) . ?
C4A C10A 1.4537(2) 17 ?
C5A C10A 1.3945(2) . ?
C5A C6A 1.4552(2) 5 ?
C6A C7A 1.3969(2) . ?
C6A C8A 1.4529(4) . ?
C7A C9A 1.4538(2) 17 ?
C9A C10A 1.4550(2) . ?
C1B C2B 1.3942(8) . ?
C1B C3B 1.4558(11) . ?
C1B C5B 1.4573(8) . ?
C2B C4B 1.4536(7) . ?
C2B C7B 1.4540(7) . ?
C3B C8B 1.406(5) 5 ?
C3B C8B 1.4051(17) . ?
C4B C9B 1.3943(7) . ?
C4B C10B 1.4501(9) 17 ?
C5B C10B 1.3950(7) . ?
C5B C6B 1.4456(10) 5 ?
C6B C7B 1.3967(7) . ?
C6B C8B 1.4530(11) . ?
C7B C9B 1.4574(9) 17 ?
C9B C10B 1.4561(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
C2A C1A C3A 120.05(5) . . ?
C2A C1A C5A 119.923(14) . . ?
C3A C1A C5A 108.00(4) . . ?
C1A C2A C7A 119.977(14) . . ?
C1A C2A C4A 120.051(14) . . ?
C7A C2A C4A 107.927(13) . . ?
C8A C3A C8A 120.12(7) . 5 ?
C8A C3A C1A 120.06(7) . . ?
C8A C3A C1A 107.80(8) 5 . ?
C9A C4A C10A 119.906(15) . 17 ?
C9A C4A C2A 120.031(14) . . ?
C10A C4A C2A 108.161(13) 17 . ?
C10A C5A C6A 119.912(15) . 5 ?
C10A C5A C1A 119.970(15) . . ?
C6A C5A C1A 107.998(15) 5 . ?
C7A C6A C8A 120.25(4) . . ?
C7A C6A C5A 119.993(18) . 9 ?
C8A C6A C5A 107.79(4) . 9 ?
C6A C7A C9A 119.892(16) . 17 ?
C6A C7A C2A 120.080(15) . . ?
C9A C7A C2A 107.962(13) 17 . ?
C3A C8A C3A 119.87(7) . 9 ?
C3A C8A C6A 119.58(7) . . ?
C3A C8A C6A 108.40(8) 9 . ?
C4A C9A C7A 120.157(15) . 21 ?
C4A C9A C10A 119.989(14) . . ?
C7A C9A C10A 108.143(14) 21 . ?
C5A C10A C4A 120.137(15) . 21 ?
C5A C10A C9A 120.035(15) . . ?
C4A C10A C9A 107.808(13) 21 . ?
C2B C1B C3B 120.56(17) . . ?
C2B C1B C5B 120.36(8) . . ?
C3B C1B C5B 106.30(19) . . ?
C1B C2B C4B 119.73(6) . . ?
C1B C2B C7B 120.07(6) . . ?
C4B C2B C7B 108.04(5) . . ?
C8B C3B C8B 121.1(3) 5 . ?
C8B C3B C1B 110.1(3) 5 . ?
C8B C3B C1B 118.4(3) . . ?
C9B C4B C10B 119.76(5) . 17 ?
C9B C4B C2B 120.10(6) . . ?
C10B C4B C2B 108.14(5) 17 . ?
C10B C5B C6B 120.02(5) . 5 ?
C10B C5B C1B 119.75(6) . . ?
C6B C5B C1B 107.72(6) 5 . ?
C7B C6B C5B 120.30(6) . 9 ?
C7B C6B C8B 118.89(18) . . ?
C5B C6B C8B 108.33(19) 9 . ?
C6B C7B C2B 120.42(6) . . ?
C6B C7B C9B 119.49(6) . 17 ?
C2B C7B C9B 107.88(5) . 17 ?
C3B C8B C3B 118.9(3) 9 . ?
C3B C8B C6B 107.5(3) 9 . ?
C3B C8B C6B 121.6(3) . . ?
C4B C9B C10B 120.13(6) . . ?
C4B C9B C7B 120.24(5) . 21 ?
C10B C9B C7B 107.90(5) . 21 ?
C5B C10B C4B 120.18(5) . 21 ?
C5B C10B C9B 119.92(5) . . ?
C4B C10B C9B 108.04(5) 21 . ?

_diffrn_measured_fraction_theta_max 1.0
_diffrn_reflns_theta_full        48.99
_diffrn_measured_fraction_theta_full 1.0
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.070


_database_code_depnum_ccdc_archive 'CCDC 930396'