# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Xian-He Bu'
_publ_contact_author_address     
;
Department of Chemistry
Nankai University
Tianjin
300071
CHINA
;

_publ_contact_author_email       BUXH@NANKAI.EDU.CN

_publ_section_title              
;
An Azido-CuII-triazolate Complex with utp-Type
Topological Network, Showing Spin-canted Antiferromagnetism
;
loop_
_publ_author_name
'Xian-He Bu.'
'Jian-Rong Li.'
'E. Carolina Sanudo'
'Ying Tao.'
'Qun Yu.'

# Attachment 'Revised_Crystallographic_Data-B702988H.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 635768'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H2 Cu N6'
_chemical_formula_sum            'C2 H2 Cu N6'
_chemical_formula_weight         173.64

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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna21
_symmetry_space_group_name_Hall  'P 2c -2n'

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

_cell_length_a                   6.7054(13)
_cell_length_b                   9.0818(18)
_cell_length_c                   8.1187(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     494.41(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3885
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.47

_exptl_crystal_description       Block
_exptl_crystal_colour            'Black Green'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             340
_exptl_absorpt_coefficient_mu    4.306
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.9102
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 10.000
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4548
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.37
_diffrn_reflns_theta_max         27.47
_reflns_number_total             1128
_reflns_number_gt                1025
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        "CrystalStructure (Rigaku/MSC'2004)"
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  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^)+(0.0180P)^2^+0.1909P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_number_reflns         1128
_refine_ls_number_parameters     91
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0560
_refine_ls_wR_factor_gt          0.0537
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.24593(4) 0.16089(3) 0.49974(13) 0.01141(11) Uani 1 1 d . . .
N1 N 0.3419(3) 0.3189(2) 0.3407(3) 0.0140(4) Uani 1 1 d . . .
N2 N 0.5255(3) 0.3857(2) 0.3424(3) 0.0134(4) Uani 1 1 d . . .
N3 N 0.3421(3) 0.4968(2) 0.1529(3) 0.0140(4) Uani 1 1 d . . .
N4 N 0.5004(4) 0.1876(3) 0.6218(3) 0.0176(5) Uani 1 1 d . . .
N5 N 0.5071(4) 0.1617(3) 0.7663(4) 0.0301(7) Uani 1 1 d . . .
N6 N 0.498(3) 0.1638(16) 0.908(2) 0.059(4) Uani 0.50 1 d P A 1
N6' N 0.541(3) 0.1073(15) 0.899(2) 0.051(4) Uani 0.50 1 d P A 2
C1 C 0.5202(4) 0.4898(3) 0.2299(4) 0.0172(7) Uani 1 1 d . . .
H1A H 0.6270 0.5516 0.2062 0.021 Uiso 1 1 calc R . .
C2 C 0.2372(4) 0.3893(4) 0.2262(4) 0.0173(6) Uani 1 1 d . . .
H2A H 0.1058 0.3666 0.1997 0.021 Uiso 1 1 calc R . .

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 0.01080(15) 0.01255(17) 0.01089(16) 0.00320(19) -0.00195(13) -0.00223(10)
N1 0.0102(10) 0.0159(11) 0.0159(12) 0.0038(9) -0.0031(10) -0.0028(8)
N2 0.0107(10) 0.0121(11) 0.0173(12) 0.0019(9) -0.0009(10) -0.0013(8)
N3 0.0107(10) 0.0161(11) 0.0152(11) 0.0040(9) -0.0005(9) 0.0002(9)
N4 0.0171(12) 0.0194(13) 0.0165(14) 0.0034(10) -0.0037(10) -0.0041(9)
N5 0.0239(15) 0.0421(17) 0.024(2) 0.0099(12) -0.0102(12) -0.0133(12)
N6 0.071(11) 0.076(12) 0.029(6) 0.028(8) -0.023(6) -0.011(7)
N6' 0.049(7) 0.072(11) 0.031(5) 0.032(7) -0.024(5) -0.015(7)
C1 0.0126(14) 0.0168(14) 0.0221(18) 0.0066(11) -0.0009(12) -0.0012(10)
C2 0.0150(14) 0.0189(15) 0.0181(15) 0.0064(12) -0.0026(11) -0.0023(11)

_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 N4 1.988(2) . ?
Cu1 N2 1.999(2) 4_455 ?
Cu1 N3 2.028(2) 3_545 ?
Cu1 N1 2.035(2) . ?
Cu1 N4 2.363(3) 4_455 ?
N1 C2 1.329(4) . ?
N1 N2 1.372(3) . ?
N2 C1 1.315(4) . ?
N2 Cu1 1.999(2) 4 ?
N3 C2 1.342(4) . ?
N3 C1 1.350(4) . ?
N3 Cu1 2.028(2) 3_554 ?
N4 N5 1.197(4) . ?
N4 Cu1 2.363(3) 4 ?
N5 N6 1.15(2) . ?
N5 N6' 1.209(16) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?

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
N4 Cu1 N2 168.24(12) . 4_455 ?
N4 Cu1 N3 91.94(10) . 3_545 ?
N2 Cu1 N3 91.22(9) 4_455 3_545 ?
N4 Cu1 N1 87.62(10) . . ?
N2 Cu1 N1 88.71(10) 4_455 . ?
N3 Cu1 N1 177.44(10) 3_545 . ?
N4 Cu1 N4 108.54(10) . 4_455 ?
N2 Cu1 N4 82.88(9) 4_455 4_455 ?
N3 Cu1 N4 88.17(10) 3_545 4_455 ?
N1 Cu1 N4 94.36(9) . 4_455 ?
C2 N1 N2 105.5(2) . . ?
C2 N1 Cu1 128.03(17) . . ?
N2 N1 Cu1 126.11(18) . . ?
C1 N2 N1 106.7(2) . . ?
C1 N2 Cu1 128.02(19) . 4 ?
N1 N2 Cu1 125.17(18) . 4 ?
C2 N3 C1 102.9(2) . . ?
C2 N3 Cu1 130.83(19) . 3_554 ?
C1 N3 Cu1 125.2(2) . 3_554 ?
N5 N4 Cu1 119.8(2) . . ?
N5 N4 Cu1 119.9(2) . 4 ?
Cu1 N4 Cu1 117.39(13) . 4 ?
N6 N5 N4 166.7(7) . . ?
N6 N5 N6' 29.0(11) . . ?
N4 N5 N6' 164.1(8) . . ?
N2 C1 N3 112.3(3) . . ?
N2 C1 H1A 123.9 . . ?
N3 C1 H1A 123.9 . . ?
N1 C2 N3 112.6(2) . . ?
N1 C2 H2A 123.7 . . ?
N3 C2 H2A 123.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Cu1 N1 C2 -167.7(3) . . . . ?
N2 Cu1 N1 C2 23.5(3) 4_455 . . . ?
N3 Cu1 N1 C2 112(2) 3_545 . . . ?
N4 Cu1 N1 C2 -59.2(3) 4_455 . . . ?
N4 Cu1 N1 N2 4.9(2) . . . . ?
N2 Cu1 N1 N2 -163.9(2) 4_455 . . . ?
N3 Cu1 N1 N2 -75(2) 3_545 . . . ?
N4 Cu1 N1 N2 113.3(2) 4_455 . . . ?
C2 N1 N2 C1 -0.3(3) . . . . ?
Cu1 N1 N2 C1 -174.26(19) . . . . ?
C2 N1 N2 Cu1 175.5(2) . . . 4 ?
Cu1 N1 N2 Cu1 1.6(3) . . . 4 ?
N2 Cu1 N4 N5 -135.6(5) 4_455 . . . ?
N3 Cu1 N4 N5 -30.1(3) 3_545 . . . ?
N1 Cu1 N4 N5 152.5(3) . . . . ?
N4 Cu1 N4 N5 58.7(2) 4_455 . . . ?
N2 Cu1 N4 Cu1 63.7(6) 4_455 . . 4 ?
N3 Cu1 N4 Cu1 169.22(13) 3_545 . . 4 ?
N1 Cu1 N4 Cu1 -8.26(14) . . . 4 ?
N4 Cu1 N4 Cu1 -102.06(19) 4_455 . . 4 ?
Cu1 N4 N5 N6 -82(5) . . . . ?
Cu1 N4 N5 N6 78(5) 4 . . . ?
Cu1 N4 N5 N6' 110(4) . . . . ?
Cu1 N4 N5 N6' -90(4) 4 . . . ?
N1 N2 C1 N3 0.2(3) . . . . ?
Cu1 N2 C1 N3 -175.6(2) 4 . . . ?
C2 N3 C1 N2 0.1(3) . . . . ?
Cu1 N3 C1 N2 169.33(19) 3_554 . . . ?
N2 N1 C2 N3 0.4(4) . . . . ?
Cu1 N1 C2 N3 174.2(2) . . . . ?
C1 N3 C2 N1 -0.3(4) . . . . ?
Cu1 N3 C2 N1 -168.7(2) 3_554 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.071