# 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
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Xiuli Wang'
_publ_contact_author_email       wangxiuli@bhu.edu.cn

_publ_section_title              
;
Encapsulation of discrete (H2O)12 clusters
in a 3-D three-fold interpenetrating metal-organic framework
host with (3,4)-connected topology
;
loop_
_publ_author_name
'Xiuli Wang.'
'Hongyan Lin.'
'Bao Mu.'
'Aixiang Tian.'
'Guocheng Liu.'

# Attachment '- complex1.cif'

data_complex1
_database_code_depnum_ccdc_archive 'CCDC 724742'
#TrackingRef '- complex1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H16 Cu N4 O6, 1.32(H2O)'
_chemical_formula_sum            'C24 H18.64 Cu N4 O7.32'
_chemical_formula_weight         543.97

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_Int_Tables_number      No.148

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   18.5636(3)
_cell_length_b                   18.5636(3)
_cell_length_c                   19.7224(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5885.9(2)
_cell_formula_units_Z            9
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8490
_cell_measurement_theta_min      2.4230
_cell_measurement_theta_max      25.9136

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2504
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18822
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         24.97
_reflns_number_total             2299
_reflns_number_gt                2022
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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^)+(0.0623P)^2^+9.9813P] 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         2299
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.181
_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 0.5000 0.01766(18) Uani 1 2 d S . .
N1 N 0.49041(13) 0.00643(13) 0.60119(12) 0.0217(5) Uani 1 1 d . . .
N2 N 0.49189(14) -0.01349(15) 0.85826(12) 0.0264(5) Uani 1 1 d . . .
H2A H 0.5168 -0.0386 0.8401 0.032 Uiso 1 1 calc R . .
C1 C 0.59982(16) 0.15591(15) 0.49146(13) 0.0198(6) Uani 1 1 d . . .
C2 C 0.63442(16) 0.24783(15) 0.48917(13) 0.0213(6) Uani 1 1 d . . .
C3 C 0.58116(15) 0.27988(16) 0.48921(13) 0.0208(6) Uani 1 1 d . . .
H3A H 0.5227 0.2434 0.4893 0.025 Uiso 1 1 calc R . .
C4 C 0.4328(2) 0.0387(2) 0.69614(15) 0.0368(7) Uani 1 1 d . . .
H4A H 0.3993 0.0602 0.7128 0.044 Uiso 1 1 calc R . .
C5 C 0.4449(2) 0.0366(2) 0.62736(14) 0.0343(7) Uani 1 1 d . . .
H5A H 0.4196 0.0576 0.5974 0.041 Uiso 1 1 calc R . .
C6 C 0.5258(2) -0.0221(2) 0.64433(15) 0.0385(8) Uani 1 1 d . . .
H6A H 0.5583 -0.0441 0.6263 0.046 Uiso 1 1 calc R . .
C7 C 0.5173(2) -0.0213(2) 0.71359(15) 0.0445(9) Uani 1 1 d . . .
H7A H 0.5441 -0.0416 0.7425 0.053 Uiso 1 1 calc R . .
C8 C 0.46947(17) 0.00935(17) 0.74073(13) 0.0256(6) Uani 1 1 d . . .
C9 C 0.45491(19) 0.01485(19) 0.81558(14) 0.0294(7) Uani 1 1 d . . .
C10 C 0.49397(16) -0.00629(17) 0.92968(15) 0.0248(6) Uani 1 1 d . . .
C11 C 0.50235(19) -0.06431(19) 0.96734(14) 0.0311(7) Uani 1 1 d . . .
H11A H 0.5039 -0.1088 0.9450 0.037 Uiso 1 1 calc R . .
C12 C 0.4915(2) 0.05852(19) 0.96262(14) 0.0321(7) Uani 1 1 d . . .
H12A H 0.4856 0.0988 0.9372 0.039 Uiso 1 1 calc R . .
O1 O 0.52031(11) 0.11199(10) 0.49113(9) 0.0210(4) Uani 1 1 d . . .
O2 O 0.64617(11) 0.12544(11) 0.49497(9) 0.0243(4) Uani 1 1 d . . .
O3 O 0.41239(17) 0.04415(17) 0.83389(11) 0.0505(7) Uani 1 1 d . . .
O1W O 0.5201(7) 0.2332(8) 0.8562(8) 0.124(5) Uani 0.33 1 d P . .
H1WA H 0.5478 0.2459 0.8928 0.149 Uiso 0.33 1 d PR . .
H1WB H 0.5664 0.2675 0.8381 0.149 Uiso 0.33 1 d PR . .
O2W O 0.5642(9) 0.2814(8) 0.9999(6) 0.114(4) Uani 0.33 1 d P . .
H2WA H 0.5562 0.2817 0.9575 0.136 Uiso 0.33 1 d PR . .
H2WB H 0.6075 0.3293 0.9998 0.136 Uiso 0.33 1 d PR . .

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 0.0222(3) 0.0152(3) 0.0142(3) 0.00044(15) -0.00018(16) 0.00839(19)
N1 0.0258(12) 0.0212(11) 0.0168(12) -0.0005(8) -0.0009(9) 0.0109(10)
N2 0.0326(13) 0.0370(13) 0.0163(12) -0.0019(10) 0.0004(9) 0.0225(11)
C1 0.0229(14) 0.0197(13) 0.0162(13) 0.0001(10) -0.0003(10) 0.0102(11)
C2 0.0218(13) 0.0195(13) 0.0218(14) 0.0003(10) -0.0002(10) 0.0097(11)
C3 0.0172(13) 0.0199(13) 0.0227(14) 0.0007(10) 0.0007(10) 0.0073(11)
C4 0.0481(19) 0.058(2) 0.0245(15) -0.0008(14) 0.0009(13) 0.0417(17)
C5 0.0477(18) 0.0536(19) 0.0206(15) 0.0022(13) -0.0017(13) 0.0397(17)
C6 0.060(2) 0.061(2) 0.0200(15) -0.0002(14) 0.0017(14) 0.0492(19)
C7 0.072(2) 0.076(2) 0.0193(15) 0.0015(15) -0.0026(15) 0.062(2)
C8 0.0305(15) 0.0298(15) 0.0184(14) -0.0003(11) -0.0004(11) 0.0166(13)
C9 0.0376(16) 0.0376(17) 0.0192(14) -0.0020(12) -0.0001(12) 0.0236(14)
C10 0.0240(14) 0.0340(15) 0.0164(14) -0.0009(11) 0.0017(10) 0.0145(12)
C11 0.0424(17) 0.0362(16) 0.0216(15) -0.0051(12) -0.0018(12) 0.0248(14)
C12 0.0448(18) 0.0353(16) 0.0224(15) 0.0007(12) -0.0021(13) 0.0246(15)
O1 0.0214(10) 0.0165(9) 0.0220(9) 0.0013(7) 0.0003(7) 0.0072(8)
O2 0.0253(10) 0.0206(10) 0.0300(10) -0.0007(7) -0.0020(8) 0.0137(8)
O3 0.0778(18) 0.0879(19) 0.0229(11) -0.0053(11) -0.0019(11) 0.0694(16)
O1W 0.079(8) 0.124(10) 0.185(14) 0.074(10) 0.025(8) 0.062(8)
O2W 0.157(12) 0.117(10) 0.076(8) 0.011(7) -0.005(8) 0.076(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 O1 1.9263(17) 10_656 ?
Cu1 O1 1.9263(17) . ?
Cu1 N1 2.012(2) 10_656 ?
Cu1 N1 2.013(2) . ?
Cu1 C1 2.545(2) . ?
Cu1 C1 2.545(2) 10_656 ?
N1 C5 1.330(4) . ?
N1 C6 1.336(4) . ?
N2 C9 1.348(4) . ?
N2 C10 1.414(4) . ?
N2 H2A 0.8800 . ?
C1 O2 1.246(3) . ?
C1 O1 1.281(3) . ?
C1 C2 1.493(3) . ?
C2 C3 1.386(4) . ?
C2 C3 1.392(4) 2_655 ?
C3 C2 1.392(4) 3_665 ?
C3 H3A 0.9500 . ?
C4 C5 1.378(4) . ?
C4 C8 1.380(4) . ?
C4 H4A 0.9500 . ?
C5 H5A 0.9500 . ?
C6 C7 1.376(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.380(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.513(4) . ?
C9 O3 1.216(3) . ?
C10 C11 1.380(4) . ?
C10 C12 1.388(4) . ?
C11 C12 1.386(4) 10_657 ?
C11 H11A 0.9500 . ?
C12 C11 1.386(4) 10_657 ?
C12 H12A 0.9500 . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8499 . ?
O2W H2WA 0.8501 . ?
O2W H2WB 0.8499 . ?

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(2) 10_656 . ?
O1 Cu1 N1 90.08(8) 10_656 10_656 ?
O1 Cu1 N1 89.92(8) . 10_656 ?
O1 Cu1 N1 89.92(8) 10_656 . ?
O1 Cu1 N1 90.08(8) . . ?
N1 Cu1 N1 180.0 10_656 . ?
O1 Cu1 C1 150.66(8) 10_656 . ?
O1 Cu1 C1 29.34(8) . . ?
N1 Cu1 C1 88.06(8) 10_656 . ?
N1 Cu1 C1 91.94(8) . . ?
O1 Cu1 C1 29.34(8) 10_656 10_656 ?
O1 Cu1 C1 150.66(8) . 10_656 ?
N1 Cu1 C1 91.94(8) 10_656 10_656 ?
N1 Cu1 C1 88.06(8) . 10_656 ?
C1 Cu1 C1 180.0 . 10_656 ?
C5 N1 C6 117.5(2) . . ?
C5 N1 Cu1 120.23(19) . . ?
C6 N1 Cu1 122.18(19) . . ?
C9 N2 C10 125.5(2) . . ?
C9 N2 H2A 117.3 . . ?
C10 N2 H2A 117.3 . . ?
O2 C1 O1 123.3(2) . . ?
O2 C1 C2 121.4(2) . . ?
O1 C1 C2 115.3(2) . . ?
O2 C1 Cu1 75.84(14) . . ?
O1 C1 Cu1 47.48(11) . . ?
C2 C1 Cu1 162.59(18) . . ?
C3 C2 C3 120.0(3) . 2_655 ?
C3 C2 C1 119.9(2) . . ?
C3 C2 C1 120.0(2) 2_655 . ?
C2 C3 C2 120.0(3) . 3_665 ?
C2 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 3_665 . ?
C5 C4 C8 119.8(3) . . ?
C5 C4 H4A 120.1 . . ?
C8 C4 H4A 120.1 . . ?
N1 C5 C4 122.7(3) . . ?
N1 C5 H5A 118.7 . . ?
C4 C5 H5A 118.7 . . ?
N1 C6 C7 123.1(3) . . ?
N1 C6 H6A 118.4 . . ?
C7 C6 H6A 118.4 . . ?
C6 C7 C8 119.4(3) . . ?
C6 C7 H7A 120.3 . . ?
C8 C7 H7A 120.3 . . ?
C7 C8 C4 117.5(3) . . ?
C7 C8 C9 125.4(3) . . ?
C4 C8 C9 117.1(3) . . ?
O3 C9 N2 124.1(3) . . ?
O3 C9 C8 119.8(3) . . ?
N2 C9 C8 116.1(2) . . ?
C11 C10 C12 119.3(3) . . ?
C11 C10 N2 118.1(2) . . ?
C12 C10 N2 122.5(3) . . ?
C10 C11 C12 120.9(3) . 10_657 ?
C10 C11 H11A 119.6 . . ?
C12 C11 H11A 119.6 10_657 . ?
C11 C12 C10 119.8(3) 10_657 . ?
C11 C12 H12A 120.1 10_657 . ?
C10 C12 H12A 120.1 . . ?
C1 O1 Cu1 103.19(15) . . ?
H1WA O1W H1WB 84.6 . . ?
H2WA O2W H2WB 94.0 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.096