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



data_global

_journal_coden_Cambridge         182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Xiao-Chun Huang'
'Dan Li'
'Xin-Jian Lin'
'Wei Luo'
'Yu-Feng Shen'

_publ_contact_author_name        'Xiao-Chun Huang'
_publ_contact_author_email       XCHUANG@STU.EDU.CN

_publ_section_title              
;
A porous coordination framework containing discrete
hollow nanotubes as rolling up of the planar sheets based on trinuclear
[Cu3(m3-O)(m-OH)(triazolate)2]+ as building blocks
;

# Attachment 'XCHuang.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 688043'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H34 Cl2 Cu9 N21 O17.50'
_chemical_formula_weight         1431.39

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P6(3)/m

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

_cell_length_a                   12.5396(3)
_cell_length_b                   12.5396(3)
_cell_length_c                   13.9133(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1894.65(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    7249
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.9

_exptl_crystal_description       cylindrical
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_exptl_absorpt_coefficient_mu    5.188
_exptl_absorpt_correction_type   'empirical used sadabs'
_exptl_absorpt_correction_T_min  0.2715
_exptl_absorpt_correction_T_max  0.4088
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(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 CCD'
_diffrn_measurement_method       '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13763
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0096
_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       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1170
_reflns_number_gt                1111
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, 1998.'
_computing_cell_refinement       'SAINT-PLUS, Ver. 6.0, 1997'
_computing_data_reduction        'SAINT-PLUS, Ver. 6.0, 1997'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP, Ver. 6.10, Bruker AXS Inc., 2000.'
_computing_publication_material  'SHELXTL-Bruker AXS Inc., 1998.'

_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^)+(0.0607P)^2^+2.8920P] 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         1170
_refine_ls_number_parameters     145
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0825
_refine_ls_wR_factor_gt          0.0813
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_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 0.21767(3) 0.42678(4) 0.14391(3) 0.01916(18) Uani 1 1 d . . .
Cu2 Cu -0.04254(5) 0.38933(5) 0.2500 0.01784(19) Uani 1 2 d S . .
Cl1 Cl 0.3333 0.6667 0.09952(9) 0.0207(3) Uani 1 3 d S . .
O1 O 0.3263(3) 0.4418(3) 0.2500 0.0212(7) Uani 1 2 d S . .
H1 H 0.3885 0.5141 0.2500 0.025 Uiso 1 2 d SR . .
O2 O 0.1355(3) 0.4622(3) 0.2500 0.0153(6) Uani 1 2 d S . .
N1 N -0.0905(2) 0.3033(2) -0.03810(19) 0.0219(6) Uani 1 1 d . . .
N2 N -0.0345(2) 0.3753(3) 0.10896(19) 0.0210(6) Uani 1 1 d . . .
N3 N 0.0633(2) 0.3748(2) 0.06607(19) 0.0216(6) Uani 1 1 d . . .
C1 C -0.1233(3) 0.3323(3) 0.0449(2) 0.0232(7) Uani 1 1 d . . .
H1A H -0.2006 0.3232 0.0560 0.028 Uiso 1 1 calc R . .
C2 C 0.0259(3) 0.3311(3) -0.0213(2) 0.0233(7) Uani 1 1 d . . .
H2A H 0.0749 0.3208 -0.0662 0.028 Uiso 1 1 calc R . .
C3 C -0.2351(4) 0.4496(4) 0.2500 0.0187(9) Uani 1 2 d S . .
O3 O -0.1448(3) 0.5572(3) 0.2500 0.0331(8) Uani 1 2 d S . .
H3A H -0.0807 0.5548 0.2500 0.050 Uiso 0.67 2 calc SPR . .
N4 N -0.2162(3) 0.3524(3) 0.2500 0.0173(7) Uani 1 2 d S . .
O1W O 0.0000 0.0000 0.4466(13) 0.086(4) Uani 0.50 3 d SPU . 1
H1WA H -0.0624 0.0017 0.4247 0.104 Uiso 0.17 1 d PR . 1
H1WB H -0.0215 -0.0737 0.4617 0.104 Uiso 0.17 1 d PR . 1
O2W O -0.0621(15) 0.1771(14) 0.2500 0.089(4) Uani 0.50 2 d SPU A 2
H2WA H -0.0523 0.1433 0.2995 0.106 Uiso 0.50 1 d PR A 2
O3W O 0.1079(14) 0.1940(14) 0.1805(14) 0.071(4) Uani 0.25 1 d PU B 3
H3WA H 0.0409 0.1826 0.1560 0.085 Uiso 0.25 1 d PR B 3
H3WB H 0.0968 0.1265 0.2039 0.085 Uiso 0.25 1 d PR B 3
O4W O 0.219(2) 0.108(2) 0.2911(19) 0.117(8) Uani 0.25 1 d PU . 4
H4WA H 0.1935 0.0720 0.2374 0.141 Uiso 0.25 1 d PR . 4
H4WB H 0.2506 0.1855 0.2831 0.141 Uiso 0.25 1 d PR . 4
O5W O 0.069(6) 0.106(5) 0.550(4) 0.15(2) Uani 0.13 1 d PU . 5
H5WA H 0.1449 0.1294 0.5554 0.184 Uiso 0.13 1 d PR . 5
H5WB H 0.0322 0.0668 0.6001 0.184 Uiso 0.13 1 d PR . 5
O6W O 0.064(4) 0.197(3) 0.2500 0.118(11) Uani 0.25 2 d SPU C 6
H6WA H 0.0065 0.2136 0.2500 0.141 Uiso 0.25 2 d SPR C 6
H6WB H 0.0545 0.1540 0.3002 0.141 Uiso 0.13 1 d PR C 6
O7W O 0.032(3) -0.075(3) 0.390(2) 0.152(10) Uani 0.25 1 d PU D 7
H7WA H -0.0432 -0.1257 0.3784 0.182 Uiso 0.25 1 d PR D 7
H7WB H 0.0565 -0.0136 0.3524 0.182 Uiso 0.25 1 d PR D 7

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 0.0196(2) 0.0321(3) 0.0087(3) -0.00341(14) -0.00081(13) 0.01501(18)
Cu2 0.0155(3) 0.0273(3) 0.0103(3) 0.000 0.000 0.0104(2)
Cl1 0.0224(4) 0.0224(4) 0.0173(7) 0.000 0.000 0.0112(2)
O1 0.0212(15) 0.0310(17) 0.0143(15) 0.000 0.000 0.0152(14)
O2 0.0143(14) 0.0224(15) 0.0093(13) 0.000 0.000 0.0093(12)
N1 0.0221(13) 0.0252(13) 0.0137(12) -0.0012(10) -0.0023(11) 0.0084(11)
N2 0.0197(13) 0.0308(14) 0.0133(14) -0.0028(11) -0.0011(10) 0.0132(11)
N3 0.0177(13) 0.0322(15) 0.0141(12) -0.0041(10) -0.0003(10) 0.0118(11)
C1 0.0223(16) 0.0335(17) 0.0141(16) -0.0035(13) -0.0024(12) 0.0143(14)
C2 0.0230(15) 0.0323(17) 0.0117(14) -0.0040(12) -0.0016(12) 0.0117(13)
C3 0.021(2) 0.024(2) 0.0102(19) 0.000 0.000 0.0101(19)
O3 0.0214(17) 0.0201(17) 0.050(2) 0.000 0.000 0.0044(14)
N4 0.0175(18) 0.0210(18) 0.0138(17) 0.000 0.000 0.0099(15)
O1W 0.072(4) 0.072(4) 0.116(9) 0.000 0.000 0.036(2)
O2W 0.100(8) 0.072(7) 0.094(8) 0.000 0.000 0.044(6)
O3W 0.071(8) 0.056(7) 0.080(8) 0.026(7) 0.003(6) 0.028(6)
O4W 0.118(11) 0.111(11) 0.109(12) 0.004(8) -0.009(8) 0.046(8)
O5W 0.15(2) 0.15(2) 0.16(2) 0.009(10) 0.004(10) 0.075(14)
O6W 0.131(14) 0.103(13) 0.126(14) 0.000 0.000 0.062(10)
O7W 0.166(13) 0.148(13) 0.150(13) 0.022(9) -0.004(9) 0.084(10)

_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 1.953(2) . ?
Cu1 O2 1.9739(19) . ?
Cu1 N1 1.984(3) 9 ?
Cu1 N3 2.021(3) . ?
Cu1 Cl1 2.6778(5) . ?
Cu1 Cu1 2.9522(7) 10_556 ?
Cu2 O2 1.944(3) . ?
Cu2 N2 1.977(3) . ?
Cu2 N2 1.977(3) 10_556 ?
Cu2 N4 1.987(4) . ?
Cl1 Cu1 2.6778(5) 5_565 ?
Cl1 Cu1 2.6778(5) 3_665 ?
O1 Cu1 1.953(2) 10_556 ?
O2 Cu1 1.9739(19) 10_556 ?
N1 C1 1.336(4) . ?
N1 C2 1.341(4) . ?
N1 Cu1 1.984(3) 11 ?
N2 C1 1.314(4) . ?
N2 N3 1.366(4) . ?
N3 C2 1.319(4) . ?
C3 O3 1.256(6) . ?
C3 N4 1.353(6) . ?
C3 N4 1.372(6) 3_565 ?
N4 C3 1.372(6) 8_456 ?
O1W O1W 1.49(4) 7_556 ?
O4W O4W 1.14(5) 10_556 ?
O5W O5W 1.81(9) 11_556 ?
O5W O5W 1.81(9) 9_556 ?

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 O2 80.23(9) . . ?
O1 Cu1 N1 99.03(11) . 9 ?
O2 Cu1 N1 178.91(11) . 9 ?
O1 Cu1 N3 161.04(11) . . ?
O2 Cu1 N3 87.11(10) . . ?
N1 Cu1 N3 93.80(11) 9 . ?
O1 Cu1 Cl1 96.08(10) . . ?
O2 Cu1 Cl1 88.28(9) . . ?
N1 Cu1 Cl1 91.01(8) 9 . ?
N3 Cu1 Cl1 97.60(8) . . ?
O1 Cu1 Cu1 40.89(7) . 10_556 ?
O2 Cu1 Cu1 41.60(6) . 10_556 ?
N1 Cu1 Cu1 137.90(8) 9 10_556 ?
N3 Cu1 Cu1 122.40(7) . 10_556 ?
Cl1 Cu1 Cu1 103.33(3) . 10_556 ?
O2 Cu2 N2 86.79(8) . . ?
O2 Cu2 N2 86.79(8) . 10_556 ?
N2 Cu2 N2 165.88(17) . 10_556 ?
O2 Cu2 N4 167.60(14) . . ?
N2 Cu2 N4 94.48(8) . . ?
N2 Cu2 N4 94.48(8) 10_556 . ?
Cu1 Cl1 Cu1 114.85(2) 5_565 3_665 ?
Cu1 Cl1 Cu1 114.85(2) 5_565 . ?
Cu1 Cl1 Cu1 114.85(2) 3_665 . ?
Cu1 O1 Cu1 98.22(14) . 10_556 ?
Cu2 O2 Cu1 120.01(10) . . ?
Cu2 O2 Cu1 120.01(10) . 10_556 ?
Cu1 O2 Cu1 96.80(12) . 10_556 ?
C1 N1 C2 102.9(3) . . ?
C1 N1 Cu1 122.6(2) . 11 ?
C2 N1 Cu1 134.0(2) . 11 ?
C1 N2 N3 106.3(3) . . ?
C1 N2 Cu2 129.7(2) . . ?
N3 N2 Cu2 121.32(19) . . ?
C2 N3 N2 105.7(3) . . ?
C2 N3 Cu1 135.4(2) . . ?
N2 N3 Cu1 118.78(19) . . ?
N2 C1 N1 112.6(3) . . ?
N3 C2 N1 112.5(3) . . ?
O3 C3 N4 119.9(4) . . ?
O3 C3 N4 119.6(4) . 3_565 ?
N4 C3 N4 120.5(4) . 3_565 ?
C3 N4 C3 119.5(4) . 8_456 ?
C3 N4 Cu2 117.1(3) . . ?
C3 N4 Cu2 123.4(3) 8_456 . ?
O5W O5W O5W 68(5) 11_556 9_556 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.120
#End of Crystallographic Information File