# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sad
_database_code_depnum_ccdc_archive 'CCDC 1037335'
_audit_update_record             
;
2014-12-03 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C16 H32 Cu3 I4 N4, Cl O4'
_chemical_formula_sum            'C16 H32 Cl Cu3 I4 N4 O4'
_chemical_formula_weight         1078.13

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'
O O 0.0106 0.0060 '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'
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           Orthorhombic
_symmetry_space_group_name_H-M   Ama2

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

_cell_length_a                   28.800(6)
_cell_length_b                   10.330(2)
_cell_length_c                   9.2214(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2743.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3159
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.41

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2016
_exptl_absorpt_coefficient_mu    6.933
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1614
_exptl_absorpt_correction_T_max  0.2097
_exptl_absorpt_process_details   SADABS

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            13019
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         27.41
_reflns_number_total             3159
_reflns_number_gt                3009
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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)+(0.0474P)²+22.9915P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_number_reflns         3159
_refine_ls_number_parameters     142
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0883
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.096
_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 0.2500 0.52167(6) 0.64753(7) 0.02928(16) Uani 1 2 d S . .
I2 I 0.336993(18) 0.29390(4) 0.37902(5) 0.03318(13) Uani 1 1 d . . .
I3 I 0.2500 0.06559(6) 0.64276(6) 0.02488(14) Uani 1 2 d S . .
Cu1 Cu 0.2500 0.29504(15) 0.4892(2) 0.0461(4) Uani 1 2 d S . .
Cu2 Cu 0.29470(3) 0.51527(8) 0.39175(14) 0.0310(2) Uani 1 1 d . . .
N1 N 0.40129(18) 0.8592(5) 0.4106(7) 0.0256(12) Uani 1 1 d . . .
N2 N 0.34297(17) 0.6705(6) 0.4014(7) 0.0235(11) Uani 1 1 d . . .
C1 C 0.4334(3) 0.9728(8) 0.4197(10) 0.039(2) Uani 1 1 d . . .
H1A H 0.4297 1.0137 0.5137 0.046 Uiso 1 1 calc R . .
H1B H 0.4247 1.0355 0.3463 0.046 Uiso 1 1 calc R . .
C2 C 0.4849(2) 0.9371(8) 0.3988(16) 0.047(2) Uani 1 1 d . . .
H2A H 0.4889 0.8916 0.3076 0.057 Uiso 1 1 calc R . .
H2B H 0.4949 0.8803 0.4765 0.057 Uiso 1 1 calc R . .
C3 C 0.3993(4) 0.8014(9) 0.2610(10) 0.044(2) Uani 1 1 d . . .
H3A H 0.4303 0.7770 0.2300 0.053 Uiso 1 1 calc R . .
H3B H 0.3873 0.8647 0.1930 0.053 Uiso 1 1 calc R . .
C4 C 0.3678(3) 0.6819(9) 0.2628(9) 0.038(2) Uani 1 1 d . . .
H4A H 0.3455 0.6879 0.1843 0.046 Uiso 1 1 calc R . .
H4B H 0.3864 0.6048 0.2473 0.046 Uiso 1 1 calc R . .
C5 C 0.3526(3) 0.9052(8) 0.4552(13) 0.045(2) Uani 1 1 d . . .
H5A H 0.3432 0.9775 0.3949 0.054 Uiso 1 1 calc R . .
H5B H 0.3530 0.9338 0.5554 0.054 Uiso 1 1 calc R . .
C6 C 0.3182(3) 0.7927(7) 0.4372(11) 0.036(2) Uani 1 1 d . . .
H6A H 0.3008 0.7813 0.5264 0.043 Uiso 1 1 calc R . .
H6B H 0.2964 0.8130 0.3604 0.043 Uiso 1 1 calc R . .
C7 C 0.4143(3) 0.7565(8) 0.5156(9) 0.0320(17) Uani 1 1 d . . .
H7A H 0.4168 0.7936 0.6119 0.038 Uiso 1 1 calc R . .
H7B H 0.4444 0.7212 0.4896 0.038 Uiso 1 1 calc R . .
C8 C 0.3782(3) 0.6478(7) 0.5168(8) 0.0278(15) Uani 1 1 d . . .
H8A H 0.3935 0.5653 0.5006 0.033 Uiso 1 1 calc R . .
H8B H 0.3631 0.6447 0.6107 0.033 Uiso 1 1 calc R . .
Cl1 Cl 0.5000 0.5000 0.3355(5) 0.0640(9) Uani 1 2 d SDU . .
O1 O 0.5000 0.5000 0.4795(12) 0.0640(9) Uani 1 2 d SDU . .
O2 O 0.4682(5) 0.5746(16) 0.2538(18) 0.0640(9) Uani 0.50 1 d PDU . .
O3 O 0.5483(4) 0.5197(17) 0.2931(18) 0.0640(9) Uani 0.50 1 d PDU . .
O4 O 0.4969(5) 0.3695(13) 0.2773(18) 0.0640(9) Uani 0.50 1 d PDU . .


_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 2.6879(13) 4 ?
I1 Cu2 2.6879(13) . ?
I1 Cu1 2.7589(19) . ?
I2 Cu2 2.5935(11) . ?
I2 Cu1 2.7037(10) . ?
I3 Cu2 2.6832(14) 5_545 ?
I3 Cu2 2.6832(14) 8_545 ?
I3 Cu1 2.7609(18) . ?
Cu1 I2 2.7037(10) 4 ?
Cu1 Cu2 2.7641(17) . ?
Cu1 Cu2 2.7641(17) 4 ?
Cu2 N2 2.124(5) . ?
Cu2 Cu2 2.5747(17) 4 ?
Cu2 I3 2.6832(13) 5_554 ?
N1 C7 1.485(10) . ?
N1 C1 1.497(9) . ?
N1 C3 1.504(12) . ?
N1 C5 1.535(9) . ?
N2 C4 1.470(10) . ?
N2 C6 1.486(10) . ?
N2 C8 1.490(9) . ?
C1 C2 1.541(10) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C2 1.562(15) 2_675 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.533(11) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.536(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.530(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
Cl1 O1 1.328(11) . ?
Cl1 O2 1.414(12) 2_665 ?
Cl1 O2 1.414(12) . ?
Cl1 O4 1.454(13) . ?
Cl1 O4 1.454(13) 2_665 ?
Cl1 O3 1.459(12) . ?
Cl1 O3 1.459(12) 2_665 ?
O2 O3 1.14(2) 2_665 ?
O2 O4 1.18(2) 2_665 ?
O3 O2 1.14(2) 2_665 ?
O3 O4 1.739(17) 2_665 ?
O4 O2 1.18(2) 2_665 ?
O4 O3 1.739(17) 2_665 ?

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 Cu2 57.23(4) 4 . ?
Cu2 I1 Cu1 60.97(4) 4 . ?
Cu2 I1 Cu1 60.97(4) . . ?
Cu2 I2 Cu1 62.87(4) . . ?
Cu2 I3 Cu2 57.34(4) 5_545 8_545 ?
Cu2 I3 Cu1 127.24(4) 5_545 . ?
Cu2 I3 Cu1 127.24(4) 8_545 . ?
I2 Cu1 I2 135.84(8) 4 . ?
I2 Cu1 I1 101.69(4) 4 . ?
I2 Cu1 I1 101.69(4) . . ?
I2 Cu1 I3 100.89(4) 4 . ?
I2 Cu1 I3 100.89(4) . . ?
I1 Cu1 I3 117.20(7) . . ?
I2 Cu1 Cu2 108.24(6) 4 . ?
I2 Cu1 Cu2 56.62(3) . . ?
I1 Cu1 Cu2 58.24(4) . . ?
I3 Cu1 Cu2 150.84(4) . . ?
I2 Cu1 Cu2 56.62(3) 4 4 ?
I2 Cu1 Cu2 108.24(6) . 4 ?
I1 Cu1 Cu2 58.24(4) . 4 ?
I3 Cu1 Cu2 150.84(4) . 4 ?
Cu2 Cu1 Cu2 55.52(5) . 4 ?
N2 Cu2 Cu2 130.87(16) . 4 ?
N2 Cu2 I2 111.11(16) . . ?
Cu2 Cu2 I2 118.01(2) 4 . ?
N2 Cu2 I3 101.75(17) . 5_554 ?
Cu2 Cu2 I3 61.33(2) 4 5_554 ?
I2 Cu2 I3 110.94(4) . 5_554 ?
N2 Cu2 I1 104.96(18) . . ?
Cu2 Cu2 I1 61.38(2) 4 . ?
I2 Cu2 I1 106.64(4) . . ?
I3 Cu2 I1 121.09(3) 5_554 . ?
N2 Cu2 Cu1 155.86(18) . . ?
Cu2 Cu2 Cu1 62.24(2) 4 . ?
I2 Cu2 Cu1 60.52(3) . . ?
I3 Cu2 Cu1 102.37(5) 5_554 . ?
I1 Cu2 Cu1 60.78(5) . . ?
C7 N1 C1 111.5(6) . . ?
C7 N1 C3 108.9(6) . . ?
C1 N1 C3 112.7(6) . . ?
C7 N1 C5 106.1(6) . . ?
C1 N1 C5 107.9(6) . . ?
C3 N1 C5 109.5(7) . . ?
C4 N2 C6 111.0(7) . . ?
C4 N2 C8 107.6(6) . . ?
C6 N2 C8 107.6(6) . . ?
C4 N2 Cu2 110.0(5) . . ?
C6 N2 Cu2 109.7(4) . . ?
C8 N2 Cu2 110.9(4) . . ?
N1 C1 C2 113.6(6) . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 C2 109.6(8) . 2_675 ?
C1 C2 H2A 109.7 . . ?
C2 C2 H2A 109.7 2_675 . ?
C1 C2 H2B 109.7 . . ?
C2 C2 H2B 109.7 2_675 . ?
H2A C2 H2B 108.2 . . ?
N1 C3 C4 109.4(7) . . ?
N1 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
N1 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
N2 C4 C3 111.2(7) . . ?
N2 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N2 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N1 C5 C6 109.0(6) . . ?
N1 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
N1 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N2 C6 C5 110.9(6) . . ?
N2 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.0 . . ?
N1 C7 C8 110.9(6) . . ?
N1 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.0 . . ?
N2 C8 C7 110.0(6) . . ?
N2 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
N2 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
O1 Cl1 O2 122.2(7) . 2_665 ?
O1 Cl1 O2 122.2(7) . . ?
O2 Cl1 O2 115.6(13) 2_665 . ?
O1 Cl1 O4 111.7(7) . . ?
O2 Cl1 O4 48.6(9) 2_665 . ?
O2 Cl1 O4 105.6(9) . . ?
O1 Cl1 O4 111.7(7) . 2_665 ?
O2 Cl1 O4 105.6(9) 2_665 2_665 ?
O2 Cl1 O4 48.6(9) . 2_665 ?
O4 Cl1 O4 136.7(14) . 2_665 ?
O1 Cl1 O3 105.5(7) . . ?
O2 Cl1 O3 46.9(9) 2_665 . ?
O2 Cl1 O3 113.5(9) . . ?
O4 Cl1 O3 95.2(9) . . ?
O4 Cl1 O3 73.3(8) 2_665 . ?
O1 Cl1 O3 105.5(7) . 2_665 ?
O2 Cl1 O3 113.5(9) 2_665 2_665 ?
O2 Cl1 O3 46.9(9) . 2_665 ?
O4 Cl1 O3 73.3(8) . 2_665 ?
O4 Cl1 O3 95.2(9) 2_665 2_665 ?
O3 Cl1 O3 149.0(14) . 2_665 ?
O3 O2 O4 135.6(15) 2_665 2_665 ?
O3 O2 Cl1 68.7(9) 2_665 . ?
O4 O2 Cl1 67.5(9) 2_665 . ?
O2 O3 Cl1 64.5(10) 2_665 . ?
O2 O3 O4 102.9(12) 2_665 2_665 ?
Cl1 O3 O4 53.2(6) . 2_665 ?
O2 O4 Cl1 63.9(10) 2_665 . ?
O2 O4 O3 109.3(12) 2_665 2_665 ?
Cl1 O4 O3 53.5(6) . 2_665 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.41
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.302
_refine_diff_density_min         -1.685
_refine_diff_density_rms         0.165
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sad
_database_code_depnum_ccdc_archive 'CCDC 1037336'
_audit_update_record             
;
2015-03-09 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C16 H32 Cu3 I4 N4, Cl O4'
_chemical_formula_sum            'C16 H32 Cl Cu3 I4 N4 O4'
_chemical_formula_weight         1078.13

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'
O O 0.0106 0.0060 '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'
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           Orthorhombic
_symmetry_space_group_name_H-M   Ama2

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

_cell_length_a                   28.536(6)
_cell_length_b                   10.276(2)
_cell_length_c                   9.2102(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2700.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3092
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      27.40

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2016
_exptl_absorpt_coefficient_mu    7.043
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1720
_exptl_absorpt_correction_T_max  0.2154
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            12864
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.40
_reflns_number_total             3092
_reflns_number_gt                3037
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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)+(0.0302P)²+48.4465P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(1)
_refine_ls_number_reflns         3092
_refine_ls_number_parameters     152
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0731
_refine_ls_wR_factor_gt          0.0729
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.117
_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 0.2500 0.51066(6) 0.64900(6) 0.01233(13) Uani 1 2 d S . .
I2 I 0.337410(15) 0.28356(4) 0.37780(5) 0.01525(11) Uani 1 1 d . . .
I3 I 0.2500 0.05724(5) 0.64361(6) 0.01030(12) Uani 1 2 d S . .
Cu1 Cu 0.2500 0.28685(12) 0.48959(15) 0.0171(3) Uani 1 2 d S . .
Cu2 Cu 0.29490(3) 0.50579(7) 0.39276(11) 0.01253(16) Uani 1 1 d . . .
N1 N 0.40146(18) 0.8539(5) 0.4131(7) 0.0134(11) Uani 1 1 d . . .
N2 N 0.34317(17) 0.6624(5) 0.4043(6) 0.0104(11) Uani 1 1 d . . .
C1 C 0.4336(2) 0.9700(7) 0.4214(8) 0.0164(15) Uani 1 1 d . . .
H1A H 0.4305 1.0094 0.5166 0.020 Uiso 1 1 calc R . .
H1B H 0.4236 1.0337 0.3501 0.020 Uiso 1 1 calc R . .
C2 C 0.4854(2) 0.9371(7) 0.3948(12) 0.0244(16) Uani 1 1 d . . .
H2A H 0.4967 0.8792 0.4703 0.029 Uiso 1 1 calc R . .
H2B H 0.4888 0.8931 0.3021 0.029 Uiso 1 1 calc R . .
C3 C 0.3975(3) 0.8021(7) 0.2602(8) 0.0189(15) Uani 1 1 d . . .
H3A H 0.4285 0.7836 0.2220 0.023 Uiso 1 1 calc R . .
H3B H 0.3828 0.8666 0.1982 0.023 Uiso 1 1 calc R . .
C4 C 0.3676(3) 0.6758(7) 0.2624(8) 0.0185(15) Uani 1 1 d . . .
H4A H 0.3447 0.6786 0.1846 0.022 Uiso 1 1 calc R . .
H4B H 0.3877 0.6010 0.2466 0.022 Uiso 1 1 calc R . .
C5 C 0.3530(2) 0.8958(7) 0.4642(9) 0.0169(14) Uani 1 1 d . . .
H5A H 0.3431 0.9727 0.4113 0.020 Uiso 1 1 calc R . .
H5B H 0.3540 0.9173 0.5668 0.020 Uiso 1 1 calc R . .
C6 C 0.3178(2) 0.7840(6) 0.4384(9) 0.0161(15) Uani 1 1 d . . .
H6A H 0.2988 0.7716 0.5245 0.019 Uiso 1 1 calc R . .
H6B H 0.2972 0.8064 0.3585 0.019 Uiso 1 1 calc R . .
C7 C 0.4175(3) 0.7440(7) 0.5130(8) 0.0136(13) Uani 1 1 d . . .
H7A H 0.4229 0.7774 0.6100 0.016 Uiso 1 1 calc R . .
H7B H 0.4466 0.7073 0.4773 0.016 Uiso 1 1 calc R . .
C8 C 0.3792(2) 0.6376(6) 0.5171(7) 0.0122(13) Uani 1 1 d . . .
H8A H 0.3933 0.5531 0.5009 0.015 Uiso 1 1 calc R . .
H8B H 0.3645 0.6368 0.6121 0.015 Uiso 1 1 calc R . .
Cl1 Cl 0.5000 0.5000 0.3185(3) 0.0133(4) Uani 1 2 d SDU . .
O1 O 0.5000 0.5000 0.4742(12) 0.051(3) Uani 1 2 d SDU . .
O2 O 0.4659(6) 0.5773(16) 0.2479(19) 0.056(4) Uani 0.50 1 d PDU . .
O3 O 0.5472(3) 0.5567(9) 0.3051(11) 0.0133(4) Uani 0.50 1 d PDU . .
O4 O 0.5029(3) 0.3674(9) 0.2632(11) 0.0133(4) Uani 0.50 1 d PDU . .


_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 2.6859(11) 4 ?
I1 Cu2 2.6859(11) . ?
I1 Cu1 2.7286(15) . ?
I2 Cu2 2.5894(10) . ?
I2 Cu1 2.6987(8) . ?
I3 Cu2 2.6809(12) 5_545 ?
I3 Cu2 2.6809(12) 8_545 ?
I3 Cu1 2.7530(14) . ?
Cu1 I2 2.6987(8) 4 ?
Cu1 Cu2 2.7384(14) . ?
Cu1 Cu2 2.7384(14) 4 ?
Cu2 N2 2.121(5) . ?
Cu2 Cu2 2.5625(16) 4 ?
Cu2 I3 2.6809(12) 5_554 ?
N1 C1 1.506(8) . ?
N1 C3 1.509(9) . ?
N1 C5 1.522(8) . ?
N1 C7 1.528(8) . ?
N2 C6 1.479(9) . ?
N2 C8 1.483(8) . ?
N2 C4 1.488(9) . ?
C1 C2 1.538(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C2 1.537(14) 2_675 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.554(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.545(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.547(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
Cl1 O2 1.414(14) . ?
Cl1 O2 1.414(14) 2_665 ?
Cl1 O1 1.433(11) . ?
Cl1 O4 1.457(9) . ?
Cl1 O4 1.457(9) 2_665 ?
Cl1 O3 1.473(9) 2_665 ?
Cl1 O3 1.473(9) . ?
O2 O4 1.065(19) 2_665 ?
O2 O3 1.521(19) 2_665 ?
O3 O2 1.521(19) 2_665 ?
O3 O4 1.674(12) 2_665 ?
O4 O2 1.065(19) 2_665 ?
O4 O3 1.674(12) 2_665 ?

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 Cu2 56.98(4) 4 . ?
Cu2 I1 Cu1 60.76(3) 4 . ?
Cu2 I1 Cu1 60.76(3) . . ?
Cu2 I2 Cu1 62.33(3) . . ?
Cu2 I3 Cu2 57.10(4) 5_545 8_545 ?
Cu2 I3 Cu1 127.60(3) 5_545 . ?
Cu2 I3 Cu1 127.60(3) 8_545 . ?
I2 Cu1 I2 135.12(6) 4 . ?
I2 Cu1 I1 102.46(3) 4 . ?
I2 Cu1 I1 102.46(3) . . ?
I2 Cu1 Cu2 108.57(4) 4 . ?
I2 Cu1 Cu2 56.88(3) . . ?
I1 Cu1 Cu2 58.85(3) . . ?
I2 Cu1 Cu2 56.88(3) 4 4 ?
I2 Cu1 Cu2 108.57(4) . 4 ?
I1 Cu1 Cu2 58.85(3) . 4 ?
Cu2 Cu1 Cu2 55.79(4) . 4 ?
I2 Cu1 I3 100.71(3) 4 . ?
I2 Cu1 I3 100.71(3) . . ?
I1 Cu1 I3 116.43(5) . . ?
Cu2 Cu1 I3 150.68(3) . . ?
Cu2 Cu1 I3 150.68(3) 4 . ?
N2 Cu2 Cu2 130.51(14) . 4 ?
N2 Cu2 I2 111.56(14) . . ?
Cu2 Cu2 I2 117.93(2) 4 . ?
N2 Cu2 I3 101.77(16) . 5_554 ?
Cu2 Cu2 I3 61.45(2) 4 5_554 ?
I2 Cu2 I3 110.63(4) . 5_554 ?
N2 Cu2 I1 104.57(16) . . ?
Cu2 Cu2 I1 61.508(19) 4 . ?
I2 Cu2 I1 106.66(4) . . ?
I3 Cu2 I1 121.36(3) 5_554 . ?
N2 Cu2 Cu1 155.62(17) . . ?
Cu2 Cu2 Cu1 62.10(2) 4 . ?
I2 Cu2 Cu1 60.79(3) . . ?
I3 Cu2 Cu1 102.54(4) 5_554 . ?
I1 Cu2 Cu1 60.39(4) . . ?
C1 N1 C3 111.8(5) . . ?
C1 N1 C5 108.2(5) . . ?
C3 N1 C5 108.7(6) . . ?
C1 N1 C7 111.9(5) . . ?
C3 N1 C7 108.9(5) . . ?
C5 N1 C7 107.2(5) . . ?
C6 N2 C8 109.6(5) . . ?
C6 N2 C4 109.7(6) . . ?
C8 N2 C4 107.9(5) . . ?
C6 N2 Cu2 109.5(4) . . ?
C8 N2 Cu2 110.8(4) . . ?
C4 N2 Cu2 109.3(4) . . ?
N1 C1 C2 113.8(6) . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C2 C2 C1 109.6(7) 2_675 . ?
C2 C2 H2A 109.8 2_675 . ?
C1 C2 H2A 109.8 . . ?
C2 C2 H2B 109.8 2_675 . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N1 C3 C4 108.9(5) . . ?
N1 C3 H3A 109.9 . . ?
C4 C3 H3A 109.9 . . ?
N1 C3 H3B 109.9 . . ?
C4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N2 C4 C3 110.2(6) . . ?
N2 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N2 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N1 C5 C6 109.4(6) . . ?
N1 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N1 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
N2 C6 C5 110.1(5) . . ?
N2 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
N2 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.2 . . ?
N1 C7 C8 109.0(5) . . ?
N1 C7 H7A 109.9 . . ?
C8 C7 H7A 109.9 . . ?
N1 C7 H7B 109.9 . . ?
C8 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N2 C8 C7 110.6(5) . . ?
N2 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
O2 Cl1 O2 125.2(15) . 2_665 ?
O2 Cl1 O1 117.4(7) . . ?
O2 Cl1 O1 117.4(7) 2_665 . ?
O2 Cl1 O4 113.8(8) . . ?
O2 Cl1 O4 43.5(8) 2_665 . ?
O1 Cl1 O4 110.5(4) . . ?
O2 Cl1 O4 43.5(8) . 2_665 ?
O2 Cl1 O4 113.8(8) 2_665 2_665 ?
O1 Cl1 O4 110.5(4) . 2_665 ?
O4 Cl1 O4 139.0(8) . 2_665 ?
O2 Cl1 O3 63.6(8) . 2_665 ?
O2 Cl1 O3 111.6(8) 2_665 2_665 ?
O1 Cl1 O3 94.8(4) . 2_665 ?
O4 Cl1 O3 69.6(5) . 2_665 ?
O4 Cl1 O3 106.8(5) 2_665 2_665 ?
O2 Cl1 O3 111.6(8) . . ?
O2 Cl1 O3 63.6(8) 2_665 . ?
O1 Cl1 O3 94.8(4) . . ?
O4 Cl1 O3 106.8(5) . . ?
O4 Cl1 O3 69.6(5) 2_665 . ?
O3 Cl1 O3 170.4(8) 2_665 . ?
O4 O2 Cl1 70.4(9) 2_665 . ?
O4 O2 O3 130.1(13) 2_665 2_665 ?
Cl1 O2 O3 60.1(7) . 2_665 ?
Cl1 O3 O2 56.3(6) . 2_665 ?
Cl1 O3 O4 54.7(4) . 2_665 ?
O2 O3 O4 97.5(8) 2_665 2_665 ?
O2 O4 Cl1 66.1(9) 2_665 . ?
O2 O4 O3 119.7(11) 2_665 2_665 ?
Cl1 O4 O3 55.6(4) . 2_665 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.40
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.917
_refine_diff_density_min         -2.482
_refine_diff_density_rms         0.192
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sad
_database_code_depnum_ccdc_archive 'CCDC 1037337'
_audit_update_record             
;
2014-12-03 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C20 H38 Br2 Cu6 I6 N6'
_chemical_formula_sum            'C20 H38 Br2 Cu6 I6 N6'
_chemical_formula_weight         1665.02

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'
Br Br -0.2901 2.4595 '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           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   14.357(3)
_cell_length_b                   13.713(3)
_cell_length_c                   20.207(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3978.2(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4461
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      27.41

_exptl_crystal_description       pillar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3048
_exptl_absorpt_coefficient_mu    9.837
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3257
_exptl_absorpt_correction_T_max  0.4218
_exptl_absorpt_process_details   SADABS

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            35899
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         27.41
_reflns_number_total             4461
_reflns_number_gt                3812
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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)+(0.0000P)²+169.9723P] 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         4461
_refine_ls_number_parameters     182
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0841
_refine_ls_wR_factor_ref         0.1711
_refine_ls_wR_factor_gt          0.1672
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_restrained_S_all      1.225
_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
I1 I 0.08237(8) 0.27758(9) 0.37608(6) 0.0531(3) Uani 1 1 d . . .
I2 I 0.37413(8) 0.28458(9) 0.28986(6) 0.0516(3) Uani 1 1 d . . .
I3 I 0.33955(9) 0.28441(9) 0.50672(6) 0.0551(3) Uani 1 1 d . . .
Br1 Br 0.26999(14) 0.02837(14) 0.38982(10) 0.0594(5) Uani 1 1 d . . .
Cu1 Cu 0.26601(18) 0.34059(15) 0.39309(12) 0.0561(6) Uani 1 1 d . . .
Cu2 Cu 0.22684(14) 0.18426(15) 0.32387(10) 0.0456(5) Uani 1 1 d . . .
Cu3 Cu 0.20480(17) 0.17938(17) 0.45512(12) 0.0561(6) Uani 1 1 d . . .
N1 N 0.1142(13) 0.0528(11) 0.1262(7) 0.063(4) Uani 1 1 d . . .
N2 N 0.1769(8) 0.1253(9) 0.2331(6) 0.038(3) Uani 1 1 d . . .
N3 N 0.1241(13) 0.1147(14) 0.5275(9) 0.073(5) Uani 1 1 d . . .
C1 C 0.0898(19) 0.0054(19) 0.0602(12) 0.089(7) Uani 1 1 d U . .
H1A H 0.1378 0.0214 0.0282 0.107 Uiso 1 1 calc R . .
H1B H 0.0895 -0.0649 0.0658 0.107 Uiso 1 1 calc R . .
C2 C 0.006(2) 0.034(2) 0.0359(13) 0.102(8) Uani 1 1 d U . .
H2A H 0.0060 0.1030 0.0265 0.123 Uiso 1 1 calc R . .
H2B H -0.0432 0.0191 0.0670 0.123 Uiso 1 1 calc R . .
C3 C 0.2133(16) 0.0154(15) 0.1394(10) 0.070(6) Uani 1 1 d . . .
H3A H 0.2543 0.0327 0.1031 0.084 Uiso 1 1 calc R . .
H3B H 0.2132 -0.0550 0.1442 0.084 Uiso 1 1 calc R . .
C4 C 0.2459(14) 0.0643(15) 0.2038(9) 0.060(5) Uani 1 1 d . . .
H4A H 0.2633 0.0140 0.2352 0.072 Uiso 1 1 calc R . .
H4B H 0.3009 0.1030 0.1945 0.072 Uiso 1 1 calc R . .
C5 C 0.0534(17) 0.0231(17) 0.1810(9) 0.076(7) Uani 1 1 d . . .
H5A H 0.0533 -0.0474 0.1853 0.091 Uiso 1 1 calc R . .
H5B H -0.0100 0.0446 0.1728 0.091 Uiso 1 1 calc R . .
C6 C 0.0910(11) 0.0703(11) 0.2446(7) 0.040(3) Uani 1 1 d . . .
H6A H 0.0441 0.1137 0.2626 0.048 Uiso 1 1 calc R . .
H6B H 0.1030 0.0197 0.2771 0.048 Uiso 1 1 calc R . .
C7 C 0.1134(14) 0.1607(11) 0.1208(8) 0.050(4) Uani 1 1 d . . .
H7A H 0.0500 0.1840 0.1157 0.060 Uiso 1 1 calc R . .
H7B H 0.1492 0.1812 0.0825 0.060 Uiso 1 1 calc R . .
C8 C 0.1562(13) 0.2023(12) 0.1838(8) 0.051(4) Uani 1 1 d . . .
H8A H 0.2133 0.2365 0.1728 0.061 Uiso 1 1 calc R . .
H8B H 0.1135 0.2492 0.2031 0.061 Uiso 1 1 calc R . .
C9 C 0.0785(11) 0.0761(11) 0.5611(8) 0.038(3) Uani 1 1 d . . .
C10 C 0.0185(14) 0.0162(14) 0.6010(11) 0.065(5) Uani 1 1 d . . .
H10A H 0.0058 -0.0437 0.5782 0.098 Uiso 1 1 calc R . .
H10B H -0.0390 0.0501 0.6091 0.098 Uiso 1 1 calc R . .
H10C H 0.0484 0.0023 0.6424 0.098 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 2.656(2) . ?
I1 Cu3 2.730(3) . ?
I1 Cu1 2.796(3) . ?
I2 Cu2 2.615(2) . ?
I2 Cu1 2.711(3) . ?
I3 Cu3 2.628(3) . ?
I3 Cu1 2.642(3) . ?
Br1 Cu2 2.594(3) . ?
Br1 Cu1 2.627(3) 8_655 ?
Br1 Cu3 2.628(3) . ?
Cu1 Cu2 2.621(3) . ?
Cu1 Br1 2.627(3) 8_665 ?
Cu1 Cu3 2.689(3) . ?
Cu2 N2 2.129(13) . ?
Cu2 Cu3 2.672(3) . ?
Cu3 N3 2.07(2) . ?
N1 C5 1.47(3) . ?
N1 C7 1.48(2) . ?
N1 C1 1.52(2) . ?
N1 C3 1.54(3) . ?
N2 C4 1.43(2) . ?
N2 C6 1.464(19) . ?
N2 C8 1.481(19) . ?
N3 C9 1.08(2) . ?
C1 C2 1.35(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C2 1.73(5) 5 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.54(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.54(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.53(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.44(2) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 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 Cu3 59.46(7) . . ?
Cu2 I1 Cu1 57.40(7) . . ?
Cu3 I1 Cu1 58.22(7) . . ?
Cu2 I2 Cu1 58.92(7) . . ?
Cu3 I3 Cu1 61.37(7) . . ?
Cu2 Br1 Cu1 140.68(11) . 8_655 ?
Cu2 Br1 Cu3 61.54(8) . . ?
Cu1 Br1 Cu3 133.61(11) 8_655 . ?
Cu2 Cu1 Br1 138.25(12) . 8_665 ?
Cu2 Cu1 I3 108.12(9) . . ?
Br1 Cu1 I3 112.72(10) 8_665 . ?
Cu2 Cu1 Cu3 60.41(8) . . ?
Br1 Cu1 Cu3 138.87(12) 8_665 . ?
I3 Cu1 Cu3 59.05(8) . . ?
Cu2 Cu1 I2 58.70(7) . . ?
Br1 Cu1 I2 111.78(10) 8_665 . ?
I3 Cu1 I2 110.93(10) . . ?
Cu3 Cu1 I2 108.23(9) . . ?
Cu2 Cu1 I1 58.61(7) . . ?
Br1 Cu1 I1 96.56(9) 8_665 . ?
I3 Cu1 I1 113.18(9) . . ?
Cu3 Cu1 I1 59.67(7) . . ?
I2 Cu1 I1 110.96(9) . . ?
N2 Cu2 Br1 102.1(3) . . ?
N2 Cu2 I2 104.2(3) . . ?
Br1 Cu2 I2 112.05(9) . . ?
N2 Cu2 Cu1 147.4(3) . . ?
Br1 Cu2 Cu1 110.41(10) . . ?
I2 Cu2 Cu1 62.38(8) . . ?
N2 Cu2 I1 105.2(3) . . ?
Br1 Cu2 I1 112.31(9) . . ?
I2 Cu2 I1 118.85(8) . . ?
Cu1 Cu2 I1 63.98(8) . . ?
N2 Cu2 Cu3 143.7(3) . . ?
Br1 Cu2 Cu3 59.85(8) . . ?
I2 Cu2 Cu3 111.71(9) . . ?
Cu1 Cu2 Cu3 61.06(8) . . ?
I1 Cu2 Cu3 61.66(7) . . ?
N3 Cu3 I3 111.5(5) . . ?
N3 Cu3 Br1 102.5(5) . . ?
I3 Cu3 Br1 111.66(10) . . ?
N3 Cu3 Cu2 141.3(5) . . ?
I3 Cu3 Cu2 107.04(9) . . ?
Br1 Cu3 Cu2 58.61(8) . . ?
N3 Cu3 Cu1 150.0(5) . . ?
I3 Cu3 Cu1 59.58(8) . . ?
Br1 Cu3 Cu1 107.30(10) . . ?
Cu2 Cu3 Cu1 58.53(8) . . ?
N3 Cu3 I1 105.4(5) . . ?
I3 Cu3 I1 115.83(9) . . ?
Br1 Cu3 I1 108.92(10) . . ?
Cu2 Cu3 I1 58.88(7) . . ?
Cu1 Cu3 I1 62.11(8) . . ?
C5 N1 C7 109.1(16) . . ?
C5 N1 C1 113.9(18) . . ?
C7 N1 C1 111.1(16) . . ?
C5 N1 C3 109.1(16) . . ?
C7 N1 C3 110.7(16) . . ?
C1 N1 C3 102.9(16) . . ?
C4 N2 C6 110.4(13) . . ?
C4 N2 C8 106.2(14) . . ?
C6 N2 C8 107.8(12) . . ?
C4 N2 Cu2 110.3(11) . . ?
C6 N2 Cu2 110.0(9) . . ?
C8 N2 Cu2 112.1(9) . . ?
C9 N3 Cu3 173.7(19) . . ?
C2 C1 N1 114(2) . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
N1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 C2 104(3) . 5 ?
C1 C2 H2A 110.9 . . ?
C2 C2 H2A 110.9 5 . ?
C1 C2 H2B 110.9 . . ?
C2 C2 H2B 110.9 5 . ?
H2A C2 H2B 108.9 . . ?
N1 C3 C4 106.5(14) . . ?
N1 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N1 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N2 C4 C3 113.3(17) . . ?
N2 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 . . ?
N2 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
N1 C5 C6 107.8(15) . . ?
N1 C5 H5A 110.2 . . ?
C6 C5 H5A 110.2 . . ?
N1 C5 H5B 110.2 . . ?
C6 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
N2 C6 C5 112.3(14) . . ?
N2 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
N2 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
N1 C7 C8 108.0(14) . . ?
N1 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
N1 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
N2 C8 C7 112.0(13) . . ?
N2 C8 H8A 109.2 . . ?
C7 C8 H8A 109.2 . . ?
N2 C8 H8B 109.2 . . ?
C7 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
N3 C9 C10 174(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.41
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         2.248
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.252
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sad
_database_code_depnum_ccdc_archive 'CCDC 1037338'
_audit_update_record             
;
2015-03-09 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C20 H38 Br2 Cu6 I6 N6'
_chemical_formula_sum            'C20 H38 Br2 Cu6 I6 N6'
_chemical_formula_weight         1665.02

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'
Br Br -0.2901 2.4595 '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           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   14.027(3)
_cell_length_b                   13.637(3)
_cell_length_c                   20.343(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3891.2(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4365
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.42

_exptl_crystal_description       pillar
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3048
_exptl_absorpt_coefficient_mu    10.057
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3174
_exptl_absorpt_correction_T_max  0.3982
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            34935
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.42
_reflns_number_total             4365
_reflns_number_gt                4105
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_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)+(0.0000P)²+209.0525P] 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         4365
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0692
_refine_ls_wR_factor_ref         0.1513
_refine_ls_wR_factor_gt          0.1499
_refine_ls_goodness_of_fit_ref   1.294
_refine_ls_restrained_S_all      1.294
_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
I1 I 0.07764(6) 0.28042(7) 0.37475(5) 0.0240(2) Uani 1 1 d . . .
I2 I 0.37784(6) 0.28863(6) 0.29233(4) 0.0230(2) Uani 1 1 d . . .
I3 I 0.34076(6) 0.28647(7) 0.50517(4) 0.0244(2) Uani 1 1 d . . .
Br1 Br 0.27106(11) 0.03174(12) 0.38857(8) 0.0326(3) Uani 1 1 d . . .
Cu1 Cu 0.26418(13) 0.34249(12) 0.39294(8) 0.0234(4) Uani 1 1 d . . .
Cu2 Cu 0.22577(12) 0.18794(12) 0.32413(8) 0.0223(4) Uani 1 1 d . . .
Cu3 Cu 0.20184(12) 0.18265(13) 0.45349(9) 0.0243(4) Uani 1 1 d . . .
N1 N 0.1264(10) 0.0519(9) 0.1250(6) 0.031(3) Uani 1 1 d . . .
N2 N 0.1802(8) 0.1291(8) 0.2334(6) 0.021(2) Uani 1 1 d . . .
N3 N 0.1228(8) 0.1185(8) 0.5234(6) 0.0223(15) Uani 1 1 d . . .
C1 C 0.1030(14) 0.0045(12) 0.0594(8) 0.040(4) Uani 1 1 d . . .
H1A H 0.1521 0.0220 0.0280 0.048 Uiso 1 1 calc R . .
H1B H 0.1043 -0.0662 0.0647 0.048 Uiso 1 1 calc R . .
C2 C 0.0085(15) 0.0335(12) 0.0321(8) 0.046(5) Uani 1 1 d . . .
H2A H 0.0085 0.1024 0.0203 0.055 Uiso 1 1 calc R . .
H2B H -0.0415 0.0222 0.0642 0.055 Uiso 1 1 calc R . .
C3 C 0.2287(11) 0.0221(12) 0.1396(7) 0.032(3) Uani 1 1 d . . .
H3A H 0.2716 0.0497 0.1071 0.038 Uiso 1 1 calc R . .
H3B H 0.2350 -0.0488 0.1388 0.038 Uiso 1 1 calc R . .
C4 C 0.2529(11) 0.0622(11) 0.2091(7) 0.030(3) Uani 1 1 d . . .
H4A H 0.2592 0.0077 0.2395 0.036 Uiso 1 1 calc R . .
H4B H 0.3136 0.0961 0.2075 0.036 Uiso 1 1 calc R . .
C5 C 0.0647(13) 0.0163(13) 0.1787(8) 0.038(4) Uani 1 1 d . . .
H5A H 0.0745 -0.0534 0.1855 0.045 Uiso 1 1 calc R . .
H5B H -0.0018 0.0270 0.1677 0.045 Uiso 1 1 calc R . .
C6 C 0.0911(10) 0.0739(10) 0.2417(7) 0.023(3) Uani 1 1 d . . .
H6A H 0.0399 0.1189 0.2524 0.028 Uiso 1 1 calc R . .
H6B H 0.0981 0.0283 0.2780 0.028 Uiso 1 1 calc R . .
C7 C 0.1182(10) 0.1617(9) 0.1206(6) 0.022(3) Uani 1 1 d . . .
H7A H 0.0518 0.1809 0.1173 0.027 Uiso 1 1 calc R . .
H7B H 0.1516 0.1856 0.0820 0.027 Uiso 1 1 calc R . .
C8 C 0.1630(11) 0.2043(10) 0.1832(7) 0.027(3) Uani 1 1 d . . .
H8A H 0.2229 0.2356 0.1721 0.032 Uiso 1 1 calc R . .
H8B H 0.1209 0.2540 0.2011 0.032 Uiso 1 1 calc R . .
C9 C 0.0772(9) 0.0788(10) 0.5579(7) 0.0223(15) Uani 1 1 d . . .
C10 C 0.0160(9) 0.0137(10) 0.5991(7) 0.0223(15) Uani 1 1 d . . .
H10A H 0.0361 -0.0532 0.5938 0.033 Uiso 1 1 calc R . .
H10B H -0.0493 0.0201 0.5856 0.033 Uiso 1 1 calc R . .
H10C H 0.0219 0.0322 0.6445 0.033 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 2.6397(19) . ?
I1 Cu3 2.716(2) . ?
I1 Cu1 2.775(2) . ?
I2 Cu2 2.6180(19) . ?
I2 Cu1 2.696(2) . ?
I3 Cu3 2.628(2) . ?
I3 Cu1 2.636(2) . ?
Br1 Cu2 2.580(2) . ?
Br1 Cu1 2.629(2) 8_655 ?
Br1 Cu3 2.631(2) . ?
Cu1 Cu2 2.587(2) . ?
Cu1 Br1 2.629(2) 8_665 ?
Cu1 Cu3 2.652(2) . ?
Cu2 N2 2.111(12) . ?
Cu2 Cu3 2.654(3) . ?
Cu3 N3 2.004(12) . ?
N1 C5 1.48(2) . ?
N1 C7 1.505(17) . ?
N1 C1 1.519(19) . ?
N1 C3 1.52(2) . ?
N2 C4 1.455(17) . ?
N2 C8 1.468(17) . ?
N2 C6 1.469(17) . ?
N3 C9 1.094(18) . ?
C1 C2 1.49(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C2 1.61(3) 5 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.554(19) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.549(19) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.534(18) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.493(18) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 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 Cu3 59.39(6) . . ?
Cu2 I1 Cu1 57.01(5) . . ?
Cu3 I1 Cu1 57.75(5) . . ?
Cu2 I2 Cu1 58.23(5) . . ?
Cu3 I3 Cu1 60.50(6) . . ?
Cu2 Br1 Cu1 141.37(8) . 8_655 ?
Cu2 Br1 Cu3 61.22(7) . . ?
Cu1 Br1 Cu3 132.95(8) 8_655 . ?
Cu2 Cu1 Br1 137.92(9) . 8_665 ?
Cu2 Cu1 I3 108.51(7) . . ?
Br1 Cu1 I3 112.98(7) 8_665 . ?
Cu2 Cu1 Cu3 60.86(7) . . ?
Br1 Cu1 Cu3 139.51(9) 8_665 . ?
I3 Cu1 Cu3 59.60(6) . . ?
Cu2 Cu1 I2 59.36(5) . . ?
Br1 Cu1 I2 110.66(7) 8_665 . ?
I3 Cu1 I2 109.73(7) . . ?
Cu3 Cu1 I2 108.88(7) . . ?
Cu2 Cu1 I1 58.86(5) . . ?
Br1 Cu1 I1 96.76(7) 8_665 . ?
I3 Cu1 I1 114.29(7) . . ?
Cu3 Cu1 I1 60.02(6) . . ?
I2 Cu1 I1 111.91(6) . . ?
N2 Cu2 Br1 101.8(3) . . ?
N2 Cu2 Cu1 147.7(3) . . ?
Br1 Cu2 Cu1 110.26(8) . . ?
N2 Cu2 I2 103.3(3) . . ?
Br1 Cu2 I2 110.97(7) . . ?
Cu1 Cu2 I2 62.40(6) . . ?
N2 Cu2 I1 106.5(3) . . ?
Br1 Cu2 I1 112.95(7) . . ?
Cu1 Cu2 I1 64.12(6) . . ?
I2 Cu2 I1 119.15(7) . . ?
N2 Cu2 Cu3 144.9(3) . . ?
Br1 Cu2 Cu3 60.33(6) . . ?
Cu1 Cu2 Cu3 60.78(7) . . ?
I2 Cu2 Cu3 111.25(7) . . ?
I1 Cu2 Cu3 61.74(6) . . ?
N3 Cu3 I3 111.2(3) . . ?
N3 Cu3 Br1 102.6(3) . . ?
I3 Cu3 Br1 110.40(8) . . ?
N3 Cu3 Cu1 150.5(3) . . ?
I3 Cu3 Cu1 59.91(6) . . ?
Br1 Cu3 Cu1 106.74(8) . . ?
N3 Cu3 Cu2 141.8(3) . . ?
I3 Cu3 Cu2 106.76(7) . . ?
Br1 Cu3 Cu2 58.45(6) . . ?
Cu1 Cu3 Cu2 58.36(6) . . ?
N3 Cu3 I1 106.1(3) . . ?
I3 Cu3 I1 116.56(7) . . ?
Br1 Cu3 I1 108.94(7) . . ?
Cu1 Cu3 I1 62.24(6) . . ?
Cu2 Cu3 I1 58.87(6) . . ?
C5 N1 C7 109.1(12) . . ?
C5 N1 C1 112.5(12) . . ?
C7 N1 C1 110.7(11) . . ?
C5 N1 C3 108.7(12) . . ?
C7 N1 C3 110.5(12) . . ?
C1 N1 C3 105.2(12) . . ?
C4 N2 C8 108.5(11) . . ?
C4 N2 C6 108.3(11) . . ?
C8 N2 C6 107.3(11) . . ?
C4 N2 Cu2 108.8(8) . . ?
C8 N2 Cu2 113.2(9) . . ?
C6 N2 Cu2 110.6(8) . . ?
C9 N3 Cu3 174.6(12) . . ?
C2 C1 N1 114.1(14) . . ?
C2 C1 H1A 108.7 . . ?
N1 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
N1 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C1 C2 C2 106.5(18) . 5 ?
C1 C2 H2A 110.4 . . ?
C2 C2 H2A 110.4 5 . ?
C1 C2 H2B 110.4 . . ?
C2 C2 H2B 110.4 5 . ?
H2A C2 H2B 108.6 . . ?
N1 C3 C4 106.8(12) . . ?
N1 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N1 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N2 C4 C3 112.2(13) . . ?
N2 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
N2 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N1 C5 C6 107.8(12) . . ?
N1 C5 H5A 110.2 . . ?
C6 C5 H5A 110.2 . . ?
N1 C5 H5B 110.2 . . ?
C6 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
N2 C6 C5 111.7(12) . . ?
N2 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
N2 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
N1 C7 C8 107.2(11) . . ?
N1 C7 H7A 110.3 . . ?
C8 C7 H7A 110.3 . . ?
N1 C7 H7B 110.3 . . ?
C8 C7 H7B 110.3 . . ?
H7A C7 H7B 108.5 . . ?
N2 C8 C7 112.4(11) . . ?
N2 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
N2 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
N3 C9 C10 172.6(15) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         3.707
_refine_diff_density_min         -1.942
_refine_diff_density_rms         0.325
