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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Bao-Hui Ye'
_publ_contact_author_email       CESYBH@MAIL.SYSU.EDU.CN

_publ_section_title              
;
Water Nanotubes Confined to Nanochannels of (10,3)-b
Net Constructed by the Binary Building Blocks via the R22(9) Synthon
;
loop_
_publ_author_name
'Bao-Hui Ye'
'Man-Li Cao'
'Ying Cui'
'Hong-Guo Hao'
'Yan-Li Niu'
;
Li-Fei Yang
;

# Attachment 'b809511f.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 689134'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H46 N13 O16 Ru'
_chemical_formula_weight         945.87

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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fddd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   10.7216(5)
_cell_length_b                   31.7838(13)
_cell_length_c                   59.500(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     20275.9(14)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4318
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7824
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8336
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_process_details   SADABS

_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  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        negligible
_diffrn_reflns_number            11517
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_sigmaI/netI    0.1488
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4318
_reflns_number_gt                2056
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.

The atoms of the DMF molecules showed physically incorrect displacement
parameters. Its displacement parameters thus had to be
restrained in order for the model to be reasonable.
;

_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)+(0.1225P)²+0.0000P] where P=(Fo²+2Fc²)/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         4318
_refine_ls_number_parameters     275
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0754
_refine_ls_wR_factor_ref         0.2368
_refine_ls_wR_factor_gt          0.2180
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.040
_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
Ru Ru 0.3750 0.3750 0.039074(15) 0.0404(4) Uani 1 2 d S . .
C1 C 0.5327(7) 0.4113(3) -0.00297(13) 0.046(2) Uani 1 1 d . . .
H1A H 0.6002 0.3920 -0.0037 0.056 Uiso 1 1 calc R . .
C2 C 0.5086(8) 0.4431(3) -0.01783(13) 0.050(2) Uani 1 1 d . . .
H2A H 0.5560 0.4498 -0.0308 0.061 Uiso 1 1 calc R . .
C3 C 0.3666(7) 0.4447(2) 0.00789(11) 0.0322(16) Uani 1 1 d . . .
C4 C 0.2602(7) 0.4498(2) 0.02170(12) 0.041(2) Uani 1 1 d . . .
C5 C 0.0973(7) 0.4704(2) 0.04073(14) 0.048(2) Uani 1 1 d . . .
H5A H 0.0272 0.4862 0.0456 0.057 Uiso 1 1 calc R . .
C6 C 0.1375(7) 0.4338(3) 0.04945(14) 0.049(2) Uani 1 1 d . . .
H6A H 0.1004 0.4194 0.0617 0.058 Uiso 1 1 calc R . .
C7 C 0.2256(7) 0.3080(2) 0.06952(13) 0.044(2) Uani 1 1 d . . .
H7A H 0.1867 0.2909 0.0584 0.053 Uiso 1 1 calc R . .
C8 C 0.2178(7) 0.3027(3) 0.09249(14) 0.049(2) Uani 1 1 d . . .
H8A H 0.1722 0.2815 0.1001 0.059 Uiso 1 1 calc R . .
C9 C 0.3351(7) 0.3573(2) 0.08589(13) 0.0389(19) Uani 1 1 d . . .
C10 C 0.5426(7) 0.1977(2) -0.02199(13) 0.045(2) Uani 1 1 d D . .
C11 C 0.5805(7) 0.1615(2) -0.03424(12) 0.0402(19) Uani 1 1 d D . .
C12 C 0.5796(7) 0.1591(2) -0.05809(13) 0.042(2) Uani 1 1 d . . .
H12A H 0.5460 0.1821 -0.0663 0.050 Uiso 1 1 calc R . .
C13 C 0.6250 0.1250 -0.07004(16) 0.039(3) Uani 1 2 d S . .
C14 C 0.6250 0.1250 -0.09483(18) 0.048(3) Uani 1 2 d S . .
C15 C 0.6250 0.1250 -0.02281(18) 0.037(2) Uani 1 2 d S . .
H15A H 0.6250 0.1250 -0.0068 0.044 Uiso 1 2 calc SR . .
C16 C 0.8750 0.1952(7) -0.1250 0.198(14) Uani 1 2 d SD . .
H16A H 0.9031 0.1991 -0.1402 0.298 Uiso 0.50 1 d PR . .
H16B H 0.8339 0.1685 -0.1237 0.298 Uiso 0.50 1 d PR . .
H16C H 0.9452 0.1960 -0.1150 0.298 Uiso 0.50 1 d PR . .
C17 C 0.708(2) 0.2414(8) -0.1017(3) 0.106 Uiso 0.50 1 d PD . .
H17A H 0.7406 0.2287 -0.0883 0.159 Uiso 0.50 1 d PR . .
H17B H 0.6229 0.2327 -0.1038 0.159 Uiso 0.50 1 d PR . .
H17C H 0.7108 0.2715 -0.1002 0.159 Uiso 0.50 1 d PR . .
C18 C 0.756(2) 0.2495(8) -0.1414(3) 0.138(11) Uiso 0.50 1 d PD . .
H18A H 0.7866 0.2347 -0.1543 0.166 Uiso 0.50 1 d PR . .
N1 N 0.4424(6) 0.4123(2) 0.01304(10) 0.0400(15) Uani 1 1 d . . .
N2 N 0.4039(6) 0.4637(2) -0.01060(10) 0.0445(17) Uani 1 1 d . . .
H2B H 0.3683 0.4855 -0.0171 0.053 Uiso 1 1 calc R . .
N3 N 0.2404(5) 0.42065(19) 0.03780(10) 0.0395(15) Uani 1 1 d . . .
N4 N 0.1759(6) 0.4808(2) 0.02347(11) 0.0452(16) Uani 1 1 d . . .
H4A H 0.1718 0.5035 0.0151 0.054 Uiso 1 1 calc R . .
N5 N 0.3003(5) 0.34273(19) 0.06561(10) 0.0388(15) Uani 1 1 d . . .
N6 N 0.2879(6) 0.3337(2) 0.10222(10) 0.0492(18) Uani 1 1 d . . .
H6B H 0.2997 0.3373 0.1167 0.059 Uiso 1 1 calc R . .
N7 N 0.783(2) 0.2279(6) -0.1209(3) 0.134(8) Uani 0.50 1 d PD . .
O1 O 0.4759(5) 0.22562(17) -0.03152(9) 0.0523(15) Uani 1 1 d . . .
O2 O 0.5775(5) 0.20109(17) -0.00130(9) 0.0524(15) Uani 1 1 d . . .
O3 O 0.5836(7) 0.15707(18) -0.10439(9) 0.071(2) Uani 1 1 d . . .
O4 O 0.6894(18) 0.2800(6) -0.1373(3) 0.137 Uiso 0.50 1 d PD . .
O1W O 0.7116(11) 0.3299(4) -0.0239(3) 0.221(7) Uani 1 1 d . . .
H1WA H 0.7773 0.3143 -0.0160 0.331 Uiso 1 1 d R . .
H1WB H 0.7443 0.3515 -0.0294 0.331 Uiso 1 1 d R . .
O2W O 0.5801(11) 0.2856(4) -0.0594(3) 0.218(7) Uani 1 1 d . . .
H2WA H 0.5644 0.2615 -0.0513 0.328 Uiso 1 1 d R . .
H2WB H 0.6177 0.3036 -0.0492 0.328 Uiso 1 1 d R . .
O3W O 0.1250 0.2176(7) 0.1250 0.207 Uiso 1 2 d S . .
H3WA H 0.1228 0.1995 0.1120 0.310 Uiso 1 1 d R . .
O4W O 0.1006(12) 0.2979(6) -0.0653(2) 0.242(7) Uani 1 1 d . . .
H4WA H 0.0843 0.2919 -0.0790 0.363 Uiso 1 1 d R . .
H4WB H 0.1813 0.2953 -0.0644 0.363 Uiso 1 1 d R . .
O5W O -0.072(2) 0.3432(8) -0.0389(4) 0.184(9) Uani 0.50 1 d P . .
H5WA H -0.0188 0.3238 -0.0474 0.275 Uiso 0.50 1 d PR . .
H5WB H -0.0753 0.3328 -0.0263 0.275 Uiso 0.50 1 d PR . .
O6W O 0.358(2) 0.3217(11) -0.0826(3) 0.208(11) Uani 0.50 1 d P . .
H6WA H 0.3591 0.3475 -0.0826 0.312 Uiso 0.50 1 d PR . .
H6WB H 0.4281 0.3151 -0.0726 0.312 Uiso 0.50 1 d PR . .


_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
Ru N5 2.046(6) . ?
Ru N5 2.046(6) 2 ?
Ru N3 2.048(6) 2 ?
Ru N3 2.048(6) . ?
Ru N1 2.081(6) 2 ?
Ru N1 2.081(6) . ?
C1 N1 1.359(9) . ?
C1 C2 1.369(7) . ?
C1 H1A 0.9500 . ?
C2 N2 1.368(9) . ?
C2 H2A 0.9500 . ?
C3 N2 1.318(9) . ?
C3 N1 1.345(9) . ?
C3 C4 1.416(8) . ?
C4 N4 1.340(9) . ?
C4 N3 1.350(9) . ?
C5 C6 1.345(8) . ?
C5 N4 1.368(8) . ?
C5 H5A 0.9500 . ?
C6 N3 1.369(9) . ?
C6 H6A 0.9500 . ?
C7 C8 1.379(8) . ?
C7 N5 1.384(9) . ?
C7 H7A 0.9500 . ?
C8 N6 1.365(9) . ?
C8 H8A 0.9500 . ?
C9 N6 1.328(9) . ?
C9 N5 1.345(9) . ?
C9 C9 1.415(8) 2 ?
C10 O1 1.272(9) . ?
C10 O2 1.291(9) . ?
C10 C11 1.421(5) . ?
C11 C12 1.421(8) . ?
C11 C15 1.428(9) . ?
C12 C13 1.384(9) . ?
C12 H12A 0.9500 . ?
C13 C12 1.384(9) 14_545 ?
C13 C14 1.475(8) . ?
C14 O3 1.249(7) 14_545 ?
C14 O3 1.249(7) . ?
C15 C11 1.428(9) 14_545 ?
C15 H15A 0.9500 . ?
C16 N7 1.453(9) 3_654 ?
C16 N7 1.453(9) . ?
C16 H16A 0.9602 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9599 . ?
C17 N7 1.463(8) . ?
C17 H17A 0.9599 . ?
C17 H17B 0.9599 . ?
C17 H17C 0.9603 . ?
C18 O4 1.227(8) . ?
C18 N7 1.430(8) . ?
C18 H18A 0.9606 . ?
N2 H2B 0.8800 . ?
N4 H4A 0.8800 . ?
N6 H6B 0.8800 . ?
O1W H1WA 0.9813 . ?
O1W H1WB 0.8375 . ?
O2W H2WA 0.9205 . ?
O2W H2WB 0.9263 . ?
O3W H3WA 0.9643 . ?
O4W H4WA 0.8541 . ?
O4W H4WB 0.8709 . ?
O5W H5WA 0.9798 . ?
O5W H5WB 0.8201 . ?
O6W H6WA 0.8201 . ?
O6W H6WB 0.9821 . ?

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
N5 Ru N5 79.0(3) . 2 ?
N5 Ru N3 87.1(2) . 2 ?
N5 Ru N3 96.2(2) 2 2 ?
N5 Ru N3 96.2(2) . . ?
N5 Ru N3 87.1(2) 2 . ?
N3 Ru N3 175.7(3) 2 . ?
N5 Ru N1 98.8(2) . 2 ?
N5 Ru N1 175.1(2) 2 2 ?
N3 Ru N1 79.2(2) 2 2 ?
N3 Ru N1 97.6(2) . 2 ?
N5 Ru N1 175.1(2) . . ?
N5 Ru N1 98.8(2) 2 . ?
N3 Ru N1 97.6(2) 2 . ?
N3 Ru N1 79.2(2) . . ?
N1 Ru N1 83.8(3) 2 . ?
N1 C1 C2 107.5(7) . . ?
N1 C1 H1A 126.3 . . ?
C2 C1 H1A 126.3 . . ?
N2 C2 C1 107.8(7) . . ?
N2 C2 H2A 126.1 . . ?
C1 C2 H2A 126.1 . . ?
N2 C3 N1 111.0(6) . . ?
N2 C3 C4 132.5(7) . . ?
N1 C3 C4 116.3(6) . . ?
N4 C4 N3 110.0(6) . . ?
N4 C4 C3 132.4(7) . . ?
N3 C4 C3 117.3(7) . . ?
C6 C5 N4 107.5(7) . . ?
C6 C5 H5A 126.3 . . ?
N4 C5 H5A 126.3 . . ?
C5 C6 N3 109.1(7) . . ?
C5 C6 H6A 125.4 . . ?
N3 C6 H6A 125.4 . . ?
C8 C7 N5 107.3(7) . . ?
C8 C7 H7A 126.3 . . ?
N5 C7 H7A 126.3 . . ?
N6 C8 C7 107.4(7) . . ?
N6 C8 H8A 126.3 . . ?
C7 C8 H8A 126.3 . . ?
N6 C9 N5 110.9(7) . . ?
N6 C9 C9 132.9(4) . 2 ?
N5 C9 C9 116.2(4) . 2 ?
O1 C10 O2 122.0(6) . . ?
O1 C10 C11 119.7(7) . . ?
O2 C10 C11 118.3(7) . . ?
C12 C11 C10 123.7(7) . . ?
C12 C11 C15 115.7(6) . . ?
C10 C11 C15 120.6(7) . . ?
C13 C12 C11 123.6(7) . . ?
C13 C12 H12A 118.2 . . ?
C11 C12 H12A 118.2 . . ?
C12 C13 C12 118.2(9) . 14_545 ?
C12 C13 C14 120.9(5) . . ?
C12 C13 C14 120.9(5) 14_545 . ?
O3 C14 O3 125.8(10) 14_545 . ?
O3 C14 C13 117.1(5) 14_545 . ?
O3 C14 C13 117.1(5) . . ?
C11 C15 C11 123.1(9) 14_545 . ?
C11 C15 H15A 118.5 14_545 . ?
C11 C15 H15A 118.5 . . ?
N7 C16 N7 89(2) 3_654 . ?
N7 C16 H16A 62.4 3_654 . ?
N7 C16 H16A 106.2 . . ?
N7 C16 H16B 163.3 3_654 . ?
N7 C16 H16B 107.9 . . ?
H16A C16 H16B 109.5 . . ?
N7 C16 H16C 63.5 3_654 . ?
N7 C16 H16C 114.2 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N7 C17 H17A 108.6 . . ?
N7 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N7 C17 H17C 110.2 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 C18 N7 109.3(8) . . ?
O4 C18 H18A 138.0 . . ?
N7 C18 H18A 112.3 . . ?
C3 N1 C1 106.8(6) . . ?
C3 N1 Ru 113.3(5) . . ?
C1 N1 Ru 139.1(5) . . ?
C3 N2 C2 107.0(6) . . ?
C3 N2 H2B 126.5 . . ?
C2 N2 H2B 126.5 . . ?
C4 N3 C6 106.0(6) . . ?
C4 N3 Ru 113.7(5) . . ?
C6 N3 Ru 140.0(5) . . ?
C4 N4 C5 107.4(6) . . ?
C4 N4 H4A 126.3 . . ?
C5 N4 H4A 126.3 . . ?
C9 N5 C7 106.5(6) . . ?
C9 N5 Ru 114.3(5) . . ?
C7 N5 Ru 139.1(5) . . ?
C9 N6 C8 107.8(7) . . ?
C9 N6 H6B 126.1 . . ?
C8 N6 H6B 126.1 . . ?
C18 N7 C16 109.8(9) . . ?
C18 N7 C17 114.3(8) . . ?
C16 N7 C17 135.7(8) . . ?
H1WA O1W H1WB 107.5 . . ?
H2WA O2W H2WB 104.5 . . ?
H4WA O4W H4WB 104.0 . . ?
H5WA O5W H5WB 104.1 . . ?
H6WA O6W H6WB 101.6 . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.121


