# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Can-Zhong Lu'
_publ_contact_author_email       CZLU@FJIRSM.AC.CN

_publ_section_title              
;
One-Pot Synthesis of Two Unique Copper(I)
Coordination Polymers: In Situ Formation of Different Ligands
from 4-aminotriazol
;
loop_
_publ_author_name
'Can-Zhong Lu'
'Fei Wang'
'Xiao-yuan Wu'
'Yi-Ming Xie'
'Rongmin Yu'
;
Qi-Sheng Zhang
;
'Zhen-Guo Zhao'

# Attachment '2.CIF'

data_2cu
_database_code_depnum_ccdc_archive 'CCDC 699394'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H10 Cu2 I N3'
_chemical_formula_sum            'C6 H10 Cu2 I N3'
_chemical_formula_weight         378.15

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I4(1)/a
_symmetry_space_group_name_Hall  -I4ad

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

_cell_length_a                   17.1338(12)
_cell_length_b                   17.1338(12)
_cell_length_c                   19.6083(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5756.4(7)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6377
_cell_measurement_theta_min      2.3773
_cell_measurement_theta_max      27.4758

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2848
_exptl_absorpt_coefficient_mu    5.065
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4797
_exptl_absorpt_correction_T_max  0.5816
_exptl_absorpt_process_details   ?

_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  Saturn70
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21036
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3302
_reflns_number_gt                2922
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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.
;

_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)+(0.0868P)²+8.9465P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    conster
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3302
_refine_ls_number_parameters     115
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.1434
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.116
_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
I1 I 0.12885(2) 0.794461(19) -0.049666(16) 0.05319(16) Uani 1 1 d . . .
Cu1 Cu 0.01748(5) 0.67400(4) -0.07142(4) 0.0646(2) Uani 1 1 d . . .
Cu2 Cu 0.19806(4) 0.61558(4) -0.10930(4) 0.0664(2) Uani 1 1 d . . .
N1 N 0.0746(2) 0.5993(2) -0.0105(2) 0.0485(9) Uani 1 1 d . . .
N2 N 0.1483(3) 0.5772(3) -0.0298(2) 0.0542(10) Uani 1 1 d . . .
N3 N 0.1219(3) 0.5188(3) 0.0671(2) 0.0548(10) Uani 1 1 d . . .
C1 C 0.0599(3) 0.5632(3) 0.0479(2) 0.0493(10) Uani 1 1 d U B .
C2 C -0.0118(4) 0.5729(4) 0.0883(3) 0.0651(14) Uani 1 1 d DU . .
H2A H -0.0378 0.5229 0.0931 0.078 Uiso 0.50 1 calc PR A 1
H2B H -0.0471 0.6082 0.0648 0.078 Uiso 0.50 1 calc PR A 1
H2C H -0.0222 0.5250 0.1130 0.078 Uiso 0.50 1 calc PR A 2
H2D H -0.0553 0.5821 0.0576 0.078 Uiso 0.50 1 calc PR A 2
C3 C 0.0078(15) 0.6059(13) 0.1593(8) 0.116(5) Uani 0.50 1 d PDU B 1
H3A H 0.0585 0.5878 0.1730 0.173 Uiso 0.50 1 calc PR B 1
H3B H -0.0305 0.5885 0.1916 0.173 Uiso 0.50 1 calc PR B 1
H3C H 0.0078 0.6619 0.1575 0.173 Uiso 0.50 1 calc PR B 1
C3' C -0.0066(15) 0.6406(11) 0.1392(10) 0.116(5) Uani 0.50 1 d PD B 2
H3'1 H -0.0455 0.6341 0.1739 0.173 Uiso 0.50 1 calc PR B 2
H3'2 H -0.0152 0.6890 0.1157 0.173 Uiso 0.50 1 calc PR B 2
H3'3 H 0.0443 0.6411 0.1597 0.173 Uiso 0.50 1 calc PR B 2
C4 C 0.1747(3) 0.5298(3) 0.0178(3) 0.0612(13) Uani 1 1 d U D .
C5 C 0.2533(5) 0.4934(5) 0.0157(5) 0.092(2) Uani 1 1 d DU . .
H5A H 0.2467 0.4376 0.0100 0.110 Uiso 0.50 1 calc PR C 3
H5B H 0.2803 0.5126 -0.0244 0.110 Uiso 0.50 1 calc PR C 3
H5C H 0.2552 0.4477 0.0449 0.110 Uiso 0.50 1 calc PR C 4
H5D H 0.2666 0.4779 -0.0305 0.110 Uiso 0.50 1 calc PR C 4
C6 C 0.3023(17) 0.506(2) 0.0735(11) 0.176(7) Uani 0.50 1 d PDU D 3
H6A H 0.3174 0.4570 0.0927 0.264 Uiso 0.50 1 calc PR D 3
H6B H 0.2744 0.5360 0.1071 0.264 Uiso 0.50 1 calc PR D 3
H6C H 0.3481 0.5345 0.0597 0.264 Uiso 0.50 1 calc PR D 3
C6' C 0.3059(17) 0.5521(16) 0.0397(15) 0.176(7) Uani 0.50 1 d PD D 4
H6'1 H 0.3442 0.5286 0.0689 0.264 Uiso 0.50 1 calc PR D 4
H6'2 H 0.2773 0.5908 0.0648 0.264 Uiso 0.50 1 calc PR D 4
H6'3 H 0.3314 0.5762 0.0016 0.264 Uiso 0.50 1 calc PR D 4


_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
I1 Cu1 2.6000(8) 6_464 ?
I1 Cu1 2.7246(8) 16_665 ?
I1 Cu1 2.8430(9) . ?
Cu1 N1 2.006(4) . ?
Cu1 I1 2.6000(8) 6_464 ?
Cu1 Cu1 2.6725(15) 6_464 ?
Cu1 I1 2.7246(8) 11_565 ?
Cu1 Cu1 2.8260(12) 16_665 ?
Cu1 Cu1 2.8261(12) 11_565 ?
Cu2 N2 1.895(4) . ?
Cu2 N3 1.897(4) 4_454 ?
N1 C1 1.326(6) . ?
N1 N2 1.371(6) . ?
N2 C4 1.317(7) . ?
N3 C4 1.338(7) . ?
N3 C1 1.360(7) . ?
N3 Cu2 1.897(4) 3 ?
C1 C2 1.472(8) . ?
C2 C3' 1.533(14) . ?
C2 C3 1.540(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3' H3'1 0.9600 . ?
C3' H3'2 0.9600 . ?
C3' H3'3 0.9600 . ?
C4 C5 1.485(9) . ?
C5 C6 1.43(2) . ?
C5 C6' 1.43(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6' H6'1 0.9600 . ?
C6' H6'2 0.9600 . ?
C6' H6'3 0.9600 . ?

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
Cu1 I1 Cu1 64.06(3) 6_464 16_665 ?
Cu1 I1 Cu1 58.61(3) 6_464 . ?
Cu1 I1 Cu1 60.96(2) 16_665 . ?
N1 Cu1 I1 120.38(12) . 6_464 ?
N1 Cu1 Cu1 137.00(13) . 6_464 ?
I1 Cu1 Cu1 65.24(3) 6_464 6_464 ?
N1 Cu1 I1 104.92(12) . 11_565 ?
I1 Cu1 I1 112.63(3) 6_464 11_565 ?
Cu1 Cu1 I1 111.216(17) 6_464 11_565 ?
N1 Cu1 Cu1 129.13(12) . 16_665 ?
I1 Cu1 Cu1 110.26(3) 6_464 16_665 ?
Cu1 Cu1 Cu1 61.782(16) 6_464 16_665 ?
I1 Cu1 Cu1 55.83(3) 11_565 16_665 ?
N1 Cu1 Cu1 161.05(13) . 11_565 ?
I1 Cu1 Cu1 60.11(2) 6_464 11_565 ?
Cu1 Cu1 Cu1 61.782(16) 6_464 11_565 ?
I1 Cu1 Cu1 61.59(3) 11_565 11_565 ?
Cu1 Cu1 Cu1 56.44(3) 16_665 11_565 ?
N1 Cu1 I1 92.65(12) . . ?
I1 Cu1 I1 118.14(3) 6_464 . ?
Cu1 Cu1 I1 56.15(3) 6_464 . ?
I1 Cu1 I1 105.46(3) 11_565 . ?
Cu1 Cu1 I1 57.45(2) 16_665 . ?
Cu1 Cu1 I1 103.55(2) 11_565 . ?
N2 Cu2 N3 162.35(19) . 4_454 ?
C1 N1 N2 106.5(4) . . ?
C1 N1 Cu1 136.0(4) . . ?
N2 N1 Cu1 117.5(3) . . ?
C4 N2 N1 107.0(4) . . ?
C4 N2 Cu2 129.9(4) . . ?
N1 N2 Cu2 123.1(3) . . ?
C4 N3 C1 104.4(4) . . ?
C4 N3 Cu2 124.3(4) . 3 ?
C1 N3 Cu2 131.0(4) . 3 ?
N1 C1 N3 110.6(4) . . ?
N1 C1 C2 124.8(5) . . ?
N3 C1 C2 124.5(4) . . ?
C1 C2 C3' 112.7(11) . . ?
C1 C2 C3 110.2(11) . . ?
C3' C2 C3 28.5(11) . . ?
C1 C2 H2A 109.6 . . ?
C3' C2 H2A 129.2 . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
C3' C2 H2B 82.7 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C1 C2 H2C 109.1 . . ?
C3' C2 H2C 109.1 . . ?
C3 C2 H2C 84.2 . . ?
H2A C2 H2C 28.2 . . ?
H2B C2 H2C 130.5 . . ?
C1 C2 H2D 109.1 . . ?
C3' C2 H2D 109.1 . . ?
C3 C2 H2D 132.0 . . ?
H2A C2 H2D 81.5 . . ?
H2B C2 H2D 29.3 . . ?
H2C C2 H2D 107.8 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C3' H3'1 109.5 . . ?
C2 C3' H3'2 109.5 . . ?
H3'1 C3' H3'2 109.5 . . ?
C2 C3' H3'3 109.5 . . ?
H3'1 C3' H3'3 109.5 . . ?
H3'2 C3' H3'3 109.5 . . ?
N2 C4 N3 111.5(5) . . ?
N2 C4 C5 123.5(6) . . ?
N3 C4 C5 125.0(5) . . ?
C6 C5 C6' 42.2(15) . . ?
C6 C5 C4 116.6(16) . . ?
C6' C5 C4 105.5(15) . . ?
C6 C5 H5A 108.2 . . ?
C6' C5 H5A 143.6 . . ?
C4 C5 H5A 108.2 . . ?
C6 C5 H5B 108.2 . . ?
C6' C5 H5B 74.2 . . ?
C4 C5 H5B 108.2 . . ?
H5A C5 H5B 107.3 . . ?
C6 C5 H5C 68.7 . . ?
C6' C5 H5C 110.6 . . ?
C4 C5 H5C 110.6 . . ?
H5A C5 H5C 43.5 . . ?
H5B C5 H5C 137.5 . . ?
C6 C5 H5D 130.2 . . ?
C6' C5 H5D 110.6 . . ?
C4 C5 H5D 110.6 . . ?
H5A C5 H5D 69.6 . . ?
H5B C5 H5D 39.2 . . ?
H5C C5 H5D 108.8 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C6' H6'1 109.5 . . ?
C5 C6' H6'2 109.5 . . ?
H6'1 C6' H6'2 109.5 . . ?
C5 C6' H6'3 109.5 . . ?
H6'1 C6' H6'3 109.5 . . ?
H6'2 C6' H6'3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.139
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.316


# Attachment '1.CIF'

data_cu
_database_code_depnum_ccdc_archive 'CCDC 699395'

_vrf_PLAT232_cu                  
;
PROBLEM: Hirshfeld Test Diff (M-X) I1 -- Cu4 .. 135.18 su
RESPONSE: The I1 atom is not covalently bonded to the Cu4 atom.

The components of the anisotropic displacement parameters along the other
covalent bonds are not equal in magnitude because of the iodine atoms. There
are some differences but there are no (substitutional) disorder, model errors
and/or over-refinement and neither are the atomic sites assigned to the
wrong atoms.

No restraints were applied on the iodine and copper atoms, and the ORTEP shows
no elongated thermal ellipsoids.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H15 Cu2 I2 N5'
_chemical_formula_sum            'C8 H15 Cu2 I2 N5'
_chemical_formula_weight         562.13

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  -P2ybc

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

_cell_length_a                   15.034(4)
_cell_length_b                   12.181(3)
_cell_length_c                   16.814(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.133(3)
_cell_angle_gamma                90.00
_cell_volume                     3010.2(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7018
_cell_measurement_theta_min      3.0683
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2096
_exptl_absorpt_coefficient_mu    6.915
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2308
_exptl_absorpt_correction_T_max  0.2768
_exptl_absorpt_process_details   ?

_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  Mercury
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21768
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6878
_reflns_number_gt                5984
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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.
;

_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)+(0.0424P)²+4.9490P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    conster
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6878
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0870
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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
I1 I 0.82021(2) 0.36211(3) 0.375685(19) 0.03685(9) Uani 1 1 d . . .
I2 I 0.62762(2) 0.63767(3) 0.38089(2) 0.04218(10) Uani 1 1 d . . .
I3 I 0.68693(2) 0.57657(3) 0.13511(2) 0.03955(9) Uani 1 1 d . . .
I4 I 0.87848(2) 0.30850(3) 0.12558(2) 0.04090(9) Uani 1 1 d . . .
Cu1 Cu 0.92659(4) 0.41071(4) 0.26744(4) 0.03609(14) Uani 1 1 d . . .
Cu2 Cu 0.75976(5) 0.55482(5) 0.32920(5) 0.05047(18) Uani 1 1 d . . .
Cu3 Cu 0.57882(4) 0.53124(5) 0.24240(4) 0.03815(14) Uani 1 1 d . . .
Cu4 Cu 0.75045(5) 0.38372(6) 0.18541(6) 0.0605(2) Uani 1 1 d . . .
N1 N 0.9227(2) 0.5780(3) 0.2629(2) 0.0247(7) Uani 1 1 d . . .
N2 N 0.8624(2) 0.6385(3) 0.2976(2) 0.0278(7) Uani 1 1 d . . .
N3 N 0.9201(2) 0.7457(3) 0.2185(2) 0.0259(7) Uani 1 1 d . . .
N4 N 0.9476(3) 0.8420(3) 0.1827(2) 0.0297(8) Uani 1 1 d . . .
N5 N 0.8127(3) 0.8200(4) 0.0835(3) 0.0501(11) Uani 1 1 d . . .
H5A H 0.7968 0.7620 0.1061 0.060 Uiso 1 1 calc R . .
H5B H 0.7787 0.8450 0.0397 0.060 Uiso 1 1 calc R . .
N6 N 0.5827(2) 0.3652(3) 0.2463(2) 0.0304(8) Uani 1 1 d . . .
N7 N 0.6434(3) 0.3047(3) 0.2117(2) 0.0321(8) Uani 1 1 d . . .
N8 N 0.5780(2) 0.1945(3) 0.2830(2) 0.0296(8) Uani 1 1 d . . .
N9 N 0.5465(3) 0.0964(3) 0.3130(2) 0.0315(8) Uani 1 1 d . . .
N10 N 0.6759(3) 0.1136(4) 0.4212(3) 0.0595(13) Uani 1 1 d . . .
H10A H 0.6935 0.1734 0.4022 0.071 Uiso 1 1 calc R . .
H10B H 0.7069 0.0861 0.4656 0.071 Uiso 1 1 calc R . .
C1 C 0.9577(3) 0.6439(3) 0.2161(3) 0.0270(8) Uani 1 1 d . . .
C2 C 0.8631(3) 0.7396(3) 0.2711(3) 0.0278(9) Uani 1 1 d . . .
C3 C 1.0280(3) 0.6142(4) 0.1692(3) 0.0380(11) Uani 1 1 d . . .
H3A H 1.0510 0.5415 0.1855 0.046 Uiso 1 1 calc R . .
H3B H 1.0784 0.6653 0.1830 0.046 Uiso 1 1 calc R . .
C4 C 0.9926(5) 0.6155(5) 0.0772(3) 0.0575(16) Uani 1 1 d . . .
H4B H 1.0409 0.5956 0.0506 0.086 Uiso 1 1 calc R . .
H4C H 0.9712 0.6878 0.0603 0.086 Uiso 1 1 calc R . .
H4A H 0.9436 0.5640 0.0628 0.086 Uiso 1 1 calc R . .
C5 C 0.8094(3) 0.8339(4) 0.2930(3) 0.0376(11) Uani 1 1 d . . .
H5C H 0.7453 0.8150 0.2805 0.045 Uiso 1 1 calc R . .
H5D H 0.8178 0.8970 0.2602 0.045 Uiso 1 1 calc R . .
C6 C 0.8374(5) 0.8643(5) 0.3824(4) 0.0557(15) Uani 1 1 d . . .
H6A H 0.8013 0.9250 0.3937 0.084 Uiso 1 1 calc R . .
H6B H 0.9005 0.8844 0.3949 0.084 Uiso 1 1 calc R . .
H6C H 0.8280 0.8025 0.4152 0.084 Uiso 1 1 calc R . .
C7 C 0.8902(3) 0.8713(4) 0.1166(3) 0.0343(10) Uani 1 1 d . . .
C8 C 0.9135(4) 0.9712(4) 0.0745(3) 0.0528(14) Uani 1 1 d . . .
H8A H 0.9701 1.0007 0.1040 0.079 Uiso 1 1 calc R . .
H8B H 0.8663 1.0250 0.0721 0.079 Uiso 1 1 calc R . .
H8C H 0.9190 0.9525 0.0203 0.079 Uiso 1 1 calc R . .
C9 C 0.5433(3) 0.2971(3) 0.2889(3) 0.0312(9) Uani 1 1 d . . .
C10 C 0.6386(3) 0.2021(4) 0.2331(3) 0.0308(9) Uani 1 1 d . . .
C11 C 0.4733(4) 0.3271(4) 0.3354(3) 0.0423(12) Uani 1 1 d . . .
H11A H 0.4236 0.2750 0.3226 0.051 Uiso 1 1 calc R . .
H11B H 0.4493 0.3990 0.3177 0.051 Uiso 1 1 calc R . .
C12 C 0.5074(5) 0.3294(6) 0.4258(4) 0.073(2) Uani 1 1 d . . .
H12A H 0.4586 0.3495 0.4517 0.110 Uiso 1 1 calc R . .
H12B H 0.5557 0.3822 0.4393 0.110 Uiso 1 1 calc R . .
H12C H 0.5298 0.2581 0.4443 0.110 Uiso 1 1 calc R . .
C13 C 0.6910(4) 0.1084(4) 0.2094(3) 0.0426(12) Uani 1 1 d . . .
H13A H 0.6809 0.0438 0.2400 0.051 Uiso 1 1 calc R . .
H13B H 0.7554 0.1255 0.2232 0.051 Uiso 1 1 calc R . .
C14 C 0.6633(5) 0.0838(5) 0.1189(4) 0.0641(17) Uani 1 1 d . . .
H14A H 0.6984 0.0232 0.1058 0.096 Uiso 1 1 calc R . .
H14B H 0.6742 0.1473 0.0884 0.096 Uiso 1 1 calc R . .
H14C H 0.5998 0.0655 0.1053 0.096 Uiso 1 1 calc R . .
C15 C 0.5990(4) 0.0623(4) 0.3810(3) 0.0394(11) Uani 1 1 d . . .
C16 C 0.5736(4) -0.0402(4) 0.4144(3) 0.0539(14) Uani 1 1 d . . .
H16A H 0.5186 -0.0677 0.3804 0.081 Uiso 1 1 calc R . .
H16B H 0.5638 -0.0277 0.4682 0.081 Uiso 1 1 calc R . .
H16C H 0.6214 -0.0930 0.4165 0.081 Uiso 1 1 calc R . .


_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
I1 Cu2 2.5785(9) . ?
I1 Cu1 2.7283(8) . ?
I2 Cu2 2.5389(8) . ?
I2 Cu3 2.6311(8) . ?
I3 Cu4 2.6089(10) . ?
I3 Cu3 2.7265(8) . ?
I4 Cu4 2.5239(9) . ?
I4 Cu1 2.6528(8) . ?
Cu1 N1 2.039(3) . ?
Cu1 N4 2.078(4) 2_745 ?
Cu1 Cu4 2.7362(12) . ?
Cu2 N2 2.012(4) . ?
Cu2 Cu3 2.8184(11) . ?
Cu3 N6 2.024(4) . ?
Cu3 N9 2.076(4) 2_655 ?
Cu4 N7 2.003(4) . ?
N1 C1 1.310(5) . ?
N1 N2 1.389(5) . ?
N2 C2 1.311(5) . ?
N3 C2 1.357(5) . ?
N3 C1 1.366(5) . ?
N3 N4 1.419(5) . ?
N4 C7 1.305(6) . ?
N4 Cu1 2.078(4) 2_755 ?
N5 C7 1.335(6) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N6 C9 1.316(6) . ?
N6 N7 1.392(5) . ?
N7 C10 1.307(6) . ?
N8 C10 1.364(6) . ?
N8 C9 1.367(5) . ?
N8 N9 1.418(5) . ?
N9 C15 1.313(6) . ?
N9 Cu3 2.076(4) 2_645 ?
N10 C15 1.362(7) . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
C1 C3 1.489(6) . ?
C2 C5 1.493(6) . ?
C3 C4 1.527(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 H4A 0.9600 . ?
C5 C6 1.520(7) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.486(7) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C11 1.481(6) . ?
C10 C13 1.488(6) . ?
C11 C12 1.499(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.521(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.453(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?

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
Cu2 I1 Cu1 79.57(2) . . ?
Cu2 I2 Cu3 66.04(3) . . ?
Cu4 I3 Cu3 80.30(2) . . ?
Cu4 I4 Cu1 63.76(3) . . ?
N1 Cu1 N4 115.72(14) . 2_745 ?
N1 Cu1 I4 115.78(10) . . ?
N4 Cu1 I4 103.12(10) 2_745 . ?
N1 Cu1 I1 103.05(10) . . ?
N4 Cu1 I1 104.78(11) 2_745 . ?
I4 Cu1 I1 114.25(3) . . ?
N1 Cu1 Cu4 94.83(10) . . ?
N4 Cu1 Cu4 149.07(10) 2_745 . ?
I4 Cu1 Cu4 55.83(2) . . ?
I1 Cu1 Cu4 70.69(3) . . ?
N2 Cu2 I2 126.02(10) . . ?
N2 Cu2 I1 107.46(10) . . ?
I2 Cu2 I1 120.62(3) . . ?
N2 Cu2 Cu3 128.72(11) . . ?
I2 Cu2 Cu3 58.55(2) . . ?
I1 Cu2 Cu3 107.73(3) . . ?
N6 Cu3 N9 114.43(15) . 2_655 ?
N6 Cu3 I2 117.57(11) . . ?
N9 Cu3 I2 105.47(10) 2_655 . ?
N6 Cu3 I3 101.95(11) . . ?
N9 Cu3 I3 103.70(11) 2_655 . ?
I2 Cu3 I3 113.06(3) . . ?
N6 Cu3 Cu2 93.85(11) . . ?
N9 Cu3 Cu2 151.59(10) 2_655 . ?
I2 Cu3 Cu2 55.41(2) . . ?
I3 Cu3 Cu2 71.17(3) . . ?
N7 Cu4 I4 128.99(11) . . ?
N7 Cu4 I3 104.34(11) . . ?
I4 Cu4 I3 117.09(3) . . ?
N7 Cu4 Cu1 133.17(12) . . ?
I4 Cu4 Cu1 60.41(3) . . ?
I3 Cu4 Cu1 107.74(3) . . ?
C1 N1 N2 107.9(3) . . ?
C1 N1 Cu1 128.6(3) . . ?
N2 N1 Cu1 122.0(2) . . ?
C2 N2 N1 107.7(3) . . ?
C2 N2 Cu2 128.8(3) . . ?
N1 N2 Cu2 116.6(2) . . ?
C2 N3 C1 107.0(3) . . ?
C2 N3 N4 127.0(3) . . ?
C1 N3 N4 125.3(3) . . ?
C7 N4 N3 112.9(4) . . ?
C7 N4 Cu1 128.0(3) . 2_755 ?
N3 N4 Cu1 118.9(3) . 2_755 ?
C7 N5 H5A 120.0 . . ?
C7 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C9 N6 N7 107.7(3) . . ?
C9 N6 Cu3 129.4(3) . . ?
N7 N6 Cu3 122.1(3) . . ?
C10 N7 N6 108.2(4) . . ?
C10 N7 Cu4 127.9(3) . . ?
N6 N7 Cu4 117.8(3) . . ?
C10 N8 C9 107.4(4) . . ?
C10 N8 N9 126.3(3) . . ?
C9 N8 N9 125.7(4) . . ?
C15 N9 N8 113.0(4) . . ?
C15 N9 Cu3 126.4(3) . 2_645 ?
N8 N9 Cu3 120.2(3) . 2_645 ?
C15 N10 H10A 120.0 . . ?
C15 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
N1 C1 N3 108.5(4) . . ?
N1 C1 C3 126.0(4) . . ?
N3 C1 C3 125.4(4) . . ?
N2 C2 N3 108.9(4) . . ?
N2 C2 C5 126.6(4) . . ?
N3 C2 C5 124.6(4) . . ?
C1 C3 C4 113.5(4) . . ?
C1 C3 H3A 108.9 . . ?
C4 C3 H3A 108.9 . . ?
C1 C3 H3B 108.9 . . ?
C4 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
H4B C4 H4A 109.5 . . ?
H4C C4 H4A 109.5 . . ?
C2 C5 C6 112.3(4) . . ?
C2 C5 H5C 109.1 . . ?
C6 C5 H5C 109.1 . . ?
C2 C5 H5D 109.1 . . ?
C6 C5 H5D 109.1 . . ?
H5C C5 H5D 107.9 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 N5 126.1(4) . . ?
N4 C7 C8 116.7(5) . . ?
N5 C7 C8 117.2(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N6 C9 N8 108.3(4) . . ?
N6 C9 C11 125.6(4) . . ?
N8 C9 C11 126.1(4) . . ?
N7 C10 N8 108.5(4) . . ?
N7 C10 C13 126.6(4) . . ?
N8 C10 C13 124.9(4) . . ?
C9 C11 C12 114.2(5) . . ?
C9 C11 H11A 108.7 . . ?
C12 C11 H11A 108.7 . . ?
C9 C11 H11B 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 C14 111.7(5) . . ?
C10 C13 H13A 109.3 . . ?
C14 C13 H13A 109.3 . . ?
C10 C13 H13B 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N9 C15 N10 125.5(5) . . ?
N9 C15 C16 116.7(5) . . ?
N10 C15 C16 117.9(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.125

