# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_100k
_database_code_depnum_ccdc_archive 'CCDC 1813315'
_audit_update_record             
;
2017-12-24 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H4 Cu3 I N8'
_chemical_formula_sum            'C8 H4 Cu3 I N8'
_chemical_formula_weight         529.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   C2/m
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   13.696(3)
_cell_length_b                   12.695(2)
_cell_length_c                   8.0211(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.512(2)
_cell_angle_gamma                90.00
_cell_volume                     1135.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4019
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    8.288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4617
_exptl_absorpt_correction_T_max  0.5988
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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 Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4019
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.10
_reflns_number_total             1050
_reflns_number_gt                1009
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0171P)²+5.9038P] 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         1050
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0181
_refine_ls_wR_factor_ref         0.0452
_refine_ls_wR_factor_gt          0.0441
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.148
_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 0.52148(3) 0.5000 0.28563(4) 0.00874(10) Uani 1 2 d S . .
Cu1 Cu 0.5000 0.31100(5) 0.5000 0.01561(15) Uani 1 2 d S . .
Cu2 Cu 0.5000 0.36858(4) 0.0000 0.01201(15) Uani 1 2 d S . .
Cu3 Cu 0.29530(5) 0.5000 0.19945(9) 0.01385(15) Uani 1 2 d S . .
N1 N 0.6673(2) 0.2823(2) 0.6813(4) 0.0108(6) Uani 1 1 d . . .
N2 N 0.7471(2) 0.3543(2) 0.8169(4) 0.0105(6) Uani 1 1 d . . .
N3 N 0.8536(2) 0.3130(2) 0.9318(4) 0.0115(6) Uani 1 1 d . . .
N4 N 0.8463(2) 0.2116(2) 0.8740(4) 0.0105(6) Uani 1 1 d . . .
C1 C 0.7303(3) 0.1948(3) 0.7189(5) 0.0094(6) Uani 1 1 d . . .
C2 C 0.6810(3) 0.0951(3) 0.6084(5) 0.0111(7) Uani 1 1 d . . .
C3 C 0.7257(4) 0.0000 0.7120(7) 0.0102(9) Uani 1 2 d S . .
H5A H 0.7861 0.0000 0.8519 0.012 Uiso 1 2 calc SR . .
C4 C 0.5892(3) 0.0948(3) 0.3971(5) 0.0125(7) Uani 1 1 d . . .
H3A H 0.5588 0.1580 0.3266 0.015 Uiso 1 1 calc R . .
C5 C 0.5443(4) 0.0000 0.2944(7) 0.0135(10) Uani 1 2 d S . .
H4A H 0.4833 0.0000 0.1548 0.016 Uiso 1 2 calc SR . .

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
I1 0.01006(16) 0.00703(16) 0.01003(15) 0.000 0.00635(13) 0.000
Cu1 0.0090(3) 0.0111(3) 0.0191(3) 0.000 0.0039(2) 0.000
Cu2 0.0090(3) 0.0085(3) 0.0157(3) 0.000 0.0056(2) 0.000
Cu3 0.0169(3) 0.0046(3) 0.0200(3) 0.000 0.0106(3) 0.000
N1 0.0109(14) 0.0068(14) 0.0124(13) -0.0005(11) 0.0054(11) -0.0002(11)
N2 0.0110(14) 0.0061(13) 0.0140(13) -0.0003(11) 0.0071(12) -0.0009(11)
N3 0.0120(14) 0.0072(14) 0.0138(13) 0.0012(11) 0.0068(11) 0.0018(11)
N4 0.0124(14) 0.0062(13) 0.0127(13) -0.0006(11) 0.0072(11) -0.0003(11)
C1 0.0112(15) 0.0088(16) 0.0107(14) 0.0036(12) 0.0077(13) 0.0006(13)
C2 0.0114(16) 0.0101(17) 0.0147(15) -0.0003(13) 0.0091(14) -0.0007(13)
C3 0.009(2) 0.012(2) 0.011(2) 0.000 0.0065(19) 0.000
C4 0.0131(16) 0.0093(16) 0.0152(16) 0.0025(13) 0.0084(14) 0.0023(13)
C5 0.015(2) 0.013(2) 0.013(2) 0.000 0.009(2) 0.000

_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 2.7085(5) . ?
I1 Cu2 2.7085(5) 5_665 ?
I1 Cu3 2.7543(9) . ?
I1 Cu1 3.0640(6) 5_666 ?
I1 Cu1 3.0640(6) . ?
Cu1 N1 1.904(3) 2_656 ?
Cu1 N1 1.904(3) . ?
Cu1 I1 3.0640(6) 5_666 ?
Cu2 N4 2.005(3) 8_454 ?
Cu2 N4 2.005(3) 7_656 ?
Cu2 I1 2.7085(5) 5_665 ?
Cu3 N2 1.920(3) 2_656 ?
Cu3 N2 1.920(3) 5_666 ?
N1 C1 1.330(4) . ?
N1 N2 1.354(4) . ?
N2 N3 1.300(4) . ?
N2 Cu3 1.920(3) 5_666 ?
N3 N4 1.352(4) . ?
N4 C1 1.350(4) . ?
N4 Cu2 2.005(3) 7_656 ?
C1 C2 1.465(5) . ?
C2 C3 1.390(4) . ?
C2 C4 1.407(4) . ?
C3 C2 1.390(4) 6 ?
C3 H5A 0.9300 . ?
C4 C5 1.384(4) . ?
C4 H3A 0.9300 . ?
C5 C4 1.384(4) 6 ?
C5 H4A 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
Cu2 I1 Cu2 76.05(2) . 5_665 ?
Cu2 I1 Cu3 103.533(13) . . ?
Cu2 I1 Cu3 103.533(13) 5_665 . ?
Cu2 I1 Cu1 163.419(13) . 5_666 ?
Cu2 I1 Cu1 89.637(18) 5_665 5_666 ?
Cu3 I1 Cu1 71.351(10) . 5_666 ?
Cu2 I1 Cu1 89.637(18) . . ?
Cu2 I1 Cu1 163.419(13) 5_665 . ?
Cu3 I1 Cu1 71.351(10) . . ?
Cu1 I1 Cu1 103.09(2) 5_666 . ?
N1 Cu1 N1 157.92(17) 2_656 . ?
N1 Cu1 I1 96.52(8) 2_656 5_666 ?
N1 Cu1 I1 100.74(8) . 5_666 ?
N1 Cu1 I1 100.74(8) 2_656 . ?
N1 Cu1 I1 96.52(8) . . ?
I1 Cu1 I1 76.91(2) 5_666 . ?
N4 Cu2 N4 118.94(16) 8_454 7_656 ?
N4 Cu2 I1 107.79(8) 8_454 . ?
N4 Cu2 I1 108.68(8) 7_656 . ?
N4 Cu2 I1 108.68(8) 8_454 5_665 ?
N4 Cu2 I1 107.79(8) 7_656 5_665 ?
I1 Cu2 I1 103.95(2) . 5_665 ?
N2 Cu3 N2 148.80(16) 2_656 5_666 ?
N2 Cu3 I1 105.60(8) 2_656 . ?
N2 Cu3 I1 105.60(8) 5_666 . ?
C1 N1 N2 105.5(3) . . ?
C1 N1 Cu1 131.9(2) . . ?
N2 N1 Cu1 122.4(2) . . ?
N3 N2 N1 110.3(3) . . ?
N3 N2 Cu3 127.4(2) . 5_666 ?
N1 N2 Cu3 121.6(2) . 5_666 ?
N2 N3 N4 108.2(3) . . ?
C1 N4 N3 106.3(3) . . ?
C1 N4 Cu2 135.5(2) . 7_656 ?
N3 N4 Cu2 117.6(2) . 7_656 ?
N1 C1 N4 109.8(3) . . ?
N1 C1 C2 125.0(3) . . ?
N4 C1 C2 125.2(3) . . ?
C3 C2 C4 119.5(3) . . ?
C3 C2 C1 120.0(3) . . ?
C4 C2 C1 120.4(3) . . ?
C2 C3 C2 120.6(4) 6 . ?
C2 C3 H5A 119.7 6 . ?
C2 C3 H5A 119.7 . . ?
C5 C4 C2 119.8(3) . . ?
C5 C4 H3A 120.1 . . ?
C2 C4 H3A 120.1 . . ?
C4 C5 C4 120.7(4) . 6 ?
C4 C5 H4A 119.6 . . ?
C4 C5 H4A 119.6 6 . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.123
####################################################################### 
# 
# 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_293k
_database_code_depnum_ccdc_archive 'CCDC 1813316'
_audit_update_record             
;
2017-12-24 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H4 Cu3 I N8'
_chemical_formula_sum            'C8 H4 Cu3 I N8'
_chemical_formula_weight         529.74

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   C2/m
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   13.790(5)
_cell_length_b                   12.700(3)
_cell_length_c                   8.1008(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.962(3)
_cell_angle_gamma                90.00
_cell_volume                     1148.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4107
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    8.193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4109
_exptl_absorpt_correction_T_max  0.5512
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_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 Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4107
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.10
_reflns_number_total             1067
_reflns_number_gt                1003
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0348P)²+2.1607P] 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         1067
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0206
_refine_ls_wR_factor_ref         0.0542
_refine_ls_wR_factor_gt          0.0534
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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 0.47762(3) 0.0000 0.24176(4) 0.01945(12) Uani 1 2 d S . .
Cu1 Cu 0.5000 0.18854(5) 0.5000 0.03482(19) Uani 1 2 d S . .
Cu2 Cu 0.5000 0.13266(5) 0.0000 0.02833(18) Uani 1 2 d S . .
Cu3 Cu 0.70370(6) 0.0000 0.61065(10) 0.03203(19) Uani 1 2 d S . .
N1 N 0.3329(2) 0.2180(2) 0.3470(4) 0.0211(6) Uani 1 1 d . . .
N2 N 0.2535(2) 0.1454(2) 0.3221(4) 0.0206(6) Uani 1 1 d . . .
N3 N 0.1468(2) 0.1868(2) 0.2244(4) 0.0225(6) Uani 1 1 d . . .
N4 N 0.1544(2) 0.2877(2) 0.1820(4) 0.0201(6) Uani 1 1 d . . .
C1 C 0.2691(3) 0.3052(3) 0.2584(5) 0.0169(6) Uani 1 1 d . . .
C2 C 0.3190(3) 0.4051(3) 0.2472(5) 0.0180(6) Uani 1 1 d . . .
C3 C 0.2748(4) 0.5000 0.2621(7) 0.0189(9) Uani 1 2 d S . .
H3A H 0.2150 0.5000 0.2823 0.023 Uiso 1 2 calc SR . .
C4 C 0.4096(3) 0.4057(3) 0.2192(5) 0.0242(7) Uani 1 1 d . . .
H4A H 0.4400 0.3425 0.2096 0.029 Uiso 1 1 calc R . .
C5 C 0.4541(5) 0.5000 0.2058(8) 0.0280(11) Uani 1 2 d S . .
H5A H 0.5146 0.5000 0.1876 0.034 Uiso 1 2 calc SR . .

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
I1 0.02003(18) 0.01737(19) 0.01878(17) 0.000 0.01018(13) 0.000
Cu1 0.0132(3) 0.0251(4) 0.0496(4) 0.000 0.0093(3) 0.000
Cu2 0.0149(3) 0.0207(3) 0.0355(3) 0.000 0.0070(3) 0.000
Cu3 0.0374(4) 0.0080(3) 0.0438(4) 0.000 0.0200(3) 0.000
N1 0.0150(13) 0.0106(14) 0.0295(14) -0.0008(11) 0.0085(12) 0.0000(11)
N2 0.0178(13) 0.0089(13) 0.0271(14) 0.0006(11) 0.0088(12) -0.0009(10)
N3 0.0182(13) 0.0126(15) 0.0309(14) 0.0040(12) 0.0111(12) 0.0014(11)
N4 0.0155(13) 0.0124(14) 0.0276(14) 0.0018(11) 0.0099(11) 0.0007(11)
C1 0.0155(15) 0.0101(16) 0.0203(14) -0.0005(12) 0.0078(12) 0.0030(12)
C2 0.0156(14) 0.0130(16) 0.0217(15) 0.0001(13) 0.0088(12) -0.0004(12)
C3 0.013(2) 0.016(2) 0.024(2) 0.000 0.0087(18) 0.000
C4 0.0242(16) 0.0162(17) 0.0320(17) -0.0026(14) 0.0164(15) 0.0032(14)
C5 0.028(3) 0.022(3) 0.040(3) 0.000 0.024(2) 0.000

_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 2.7348(6) 5_655 ?
I1 Cu2 2.7348(6) . ?
I1 Cu3 2.7762(10) . ?
I1 Cu1 3.0736(8) . ?
I1 Cu1 3.0736(8) 5_656 ?
Cu1 N1 1.906(3) 2_656 ?
Cu1 N1 1.906(3) . ?
Cu1 I1 3.0736(8) 5_656 ?
Cu2 N4 2.010(3) 8 ?
Cu2 N4 2.010(3) 7 ?
Cu2 I1 2.7348(6) 5_655 ?
Cu3 N2 1.918(3) 2_656 ?
Cu3 N2 1.918(3) 5_656 ?
N1 C1 1.332(4) . ?
N1 N2 1.352(4) . ?
N2 N3 1.304(4) . ?
N2 Cu3 1.918(3) 5_656 ?
N3 N4 1.347(4) . ?
N4 C1 1.337(4) . ?
N4 Cu2 2.010(3) 7 ?
C1 C2 1.470(4) . ?
C2 C3 1.387(4) . ?
C2 C4 1.395(5) . ?
C3 C2 1.387(4) 6_565 ?
C3 H3A 0.9300 . ?
C4 C5 1.378(4) . ?
C4 H4A 0.9300 . ?
C5 C4 1.378(4) 6_565 ?
C5 H5A 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
Cu2 I1 Cu2 76.06(3) 5_655 . ?
Cu2 I1 Cu3 104.07(3) 5_655 . ?
Cu2 I1 Cu3 104.07(3) . . ?
Cu2 I1 Cu1 163.518(15) 5_655 . ?
Cu2 I1 Cu1 89.94(2) . . ?
Cu3 I1 Cu1 70.544(17) . . ?
Cu2 I1 Cu1 89.94(2) 5_655 5_656 ?
Cu2 I1 Cu1 163.518(15) . 5_656 ?
Cu3 I1 Cu1 70.544(17) . 5_656 ?
Cu1 I1 Cu1 102.35(3) . 5_656 ?
N1 Cu1 N1 157.36(18) 2_656 . ?
N1 Cu1 I1 101.26(9) 2_656 . ?
N1 Cu1 I1 96.35(9) . . ?
N1 Cu1 I1 96.35(9) 2_656 5_656 ?
N1 Cu1 I1 101.26(9) . 5_656 ?
I1 Cu1 I1 77.65(3) . 5_656 ?
N4 Cu2 N4 119.60(16) 8 7 ?
N4 Cu2 I1 108.59(8) 8 5_655 ?
N4 Cu2 I1 107.51(8) 7 5_655 ?
N4 Cu2 I1 107.51(8) 8 . ?
N4 Cu2 I1 108.59(8) 7 . ?
I1 Cu2 I1 103.94(3) 5_655 . ?
N2 Cu3 N2 148.71(16) 2_656 5_656 ?
N2 Cu3 I1 105.63(8) 2_656 . ?
N2 Cu3 I1 105.63(8) 5_656 . ?
C1 N1 N2 105.4(3) . . ?
C1 N1 Cu1 132.6(2) . . ?
N2 N1 Cu1 121.8(2) . . ?
N3 N2 N1 110.0(3) . . ?
N3 N2 Cu3 127.6(2) . 5_656 ?
N1 N2 Cu3 121.8(2) . 5_656 ?
N2 N3 N4 108.0(3) . . ?
C1 N4 N3 106.8(3) . . ?
C1 N4 Cu2 135.4(2) . 7 ?
N3 N4 Cu2 117.3(2) . 7 ?
N1 C1 N4 109.8(3) . . ?
N1 C1 C2 124.5(3) . . ?
N4 C1 C2 125.7(3) . . ?
C3 C2 C4 119.3(3) . . ?
C3 C2 C1 119.9(3) . . ?
C4 C2 C1 120.7(3) . . ?
C2 C3 C2 120.6(4) 6_565 . ?
C2 C3 H3A 119.7 6_565 . ?
C2 C3 H3A 119.7 . . ?
C5 C4 C2 120.0(3) . . ?
C5 C4 H4A 120.0 . . ?
C2 C4 H4A 120.0 . . ?
C4 C5 C4 120.6(5) . 6_565 ?
C4 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 6_565 . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.117
####################################################################### 
# 
# 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_220k
_database_code_depnum_ccdc_archive 'CCDC 1813317'
_audit_update_record             
;
2017-12-24 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H4 Cu3 I N8'
_chemical_formula_sum            'C8 H4 Cu3 I N8'
_chemical_formula_weight         529.74

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   C2/m
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   13.766(2)
_cell_length_b                   12.7157(18)
_cell_length_c                   8.0750(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.800(2)
_cell_angle_gamma                90.00
_cell_volume                     1146.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    4030
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    8.207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4104
_exptl_absorpt_correction_T_max  0.5507
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      220(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 Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4030
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.10
_reflns_number_total             1056
_reflns_number_gt                1001
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0268P)²+4.2455P] 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         1056
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0498
_refine_ls_wR_factor_gt          0.0491
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_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 0.52202(3) 0.0000 0.28615(4) 0.01446(11) Uani 1 2 d S . .
Cu1 Cu 0.5000 0.18865(5) 0.5000 0.02647(18) Uani 1 2 d S . .
Cu2 Cu 0.5000 0.13221(5) 0.0000 0.02089(16) Uani 1 2 d S . .
Cu3 Cu 0.29587(6) 0.0000 0.20183(11) 0.02399(17) Uani 1 2 d S . .
N1 N 0.6672(2) 0.2179(2) 0.6814(4) 0.0163(6) Uani 1 1 d . . .
N2 N 0.7464(2) 0.1456(2) 0.8155(5) 0.0167(6) Uani 1 1 d . . .
N3 N 0.8535(2) 0.1870(2) 0.9316(4) 0.0177(6) Uani 1 1 d . . .
N4 N 0.8458(2) 0.2880(2) 0.8734(4) 0.0157(6) Uani 1 1 d . . .
C1 C 0.7309(3) 0.3050(3) 0.7199(5) 0.0138(7) Uani 1 1 d . . .
C2 C 0.6807(3) 0.4053(3) 0.6082(5) 0.0151(7) Uani 1 1 d . . .
C3 C 0.7253(4) 0.5000 0.7122(7) 0.0147(9) Uani 1 2 d S . .
H5A H 0.7852 0.5000 0.8520 0.018 Uiso 1 2 calc SR . .
C4 C 0.5903(3) 0.4053(3) 0.3998(5) 0.0189(7) Uani 1 1 d . . .
H3A H 0.5601 0.3420 0.3300 0.023 Uiso 1 1 calc R . .
C5 C 0.5451(5) 0.5000 0.2957(8) 0.0211(11) Uani 1 2 d S . .
H4A H 0.4846 0.5000 0.1562 0.025 Uiso 1 2 calc SR . .

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
I1 0.01501(17) 0.01310(17) 0.01610(18) 0.000 0.00957(14) 0.000
Cu1 0.0104(3) 0.0192(3) 0.0344(4) 0.000 0.0044(3) 0.000
Cu2 0.0116(3) 0.0154(3) 0.0281(4) 0.000 0.0074(3) 0.000
Cu3 0.0284(3) 0.0063(3) 0.0357(4) 0.000 0.0179(3) 0.000
N1 0.0124(13) 0.0096(13) 0.0210(15) -0.0007(12) 0.0065(12) -0.0003(11)
N2 0.0142(14) 0.0085(13) 0.0239(16) 0.0009(11) 0.0092(13) 0.0005(11)
N3 0.0146(14) 0.0116(14) 0.0210(16) 0.0008(12) 0.0071(12) -0.0012(11)
N4 0.0141(14) 0.0097(13) 0.0192(15) 0.0001(12) 0.0075(12) -0.0008(11)
C1 0.0149(15) 0.0087(16) 0.0170(17) -0.0031(13) 0.0089(14) -0.0016(12)
C2 0.0130(15) 0.0100(16) 0.0211(18) 0.0011(14) 0.0093(14) 0.0018(13)
C3 0.008(2) 0.015(2) 0.017(2) 0.000 0.0050(19) 0.000
C4 0.0197(17) 0.0122(17) 0.0213(18) -0.0045(14) 0.0100(15) -0.0024(14)
C5 0.021(2) 0.020(3) 0.015(3) 0.000 0.007(2) 0.000

_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 2.7273(5) 5_655 ?
I1 Cu2 2.7273(5) . ?
I1 Cu3 2.7706(8) . ?
I1 Cu1 3.0726(6) . ?
I1 Cu1 3.0726(6) 5_656 ?
Cu1 N1 1.907(3) . ?
Cu1 N1 1.907(3) 2_656 ?
Cu1 I1 3.0726(6) 5_656 ?
Cu2 N4 2.011(3) 7_656 ?
Cu2 N4 2.011(3) 8_454 ?
Cu2 I1 2.7273(5) 5_655 ?
Cu3 N2 1.921(3) 5_656 ?
Cu3 N2 1.921(3) 2_656 ?
N1 C1 1.332(4) . ?
N1 N2 1.351(4) . ?
N2 N3 1.308(4) . ?
N2 Cu3 1.921(3) 5_656 ?
N3 N4 1.351(4) . ?
N4 C1 1.338(4) . ?
N4 Cu2 2.011(3) 7_656 ?
C1 C2 1.479(5) . ?
C2 C3 1.389(4) . ?
C2 C4 1.389(5) . ?
C3 C2 1.389(4) 6_565 ?
C3 H5A 0.9300 . ?
C4 C5 1.390(4) . ?
C4 H3A 0.9300 . ?
C5 C4 1.390(4) 6_565 ?
C5 H4A 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
Cu2 I1 Cu2 76.11(2) 5_655 . ?
Cu2 I1 Cu3 103.873(14) 5_655 . ?
Cu2 I1 Cu3 103.873(14) . . ?
Cu2 I1 Cu1 163.501(15) 5_655 . ?
Cu2 I1 Cu1 89.788(16) . . ?
Cu3 I1 Cu1 70.853(10) . . ?
Cu2 I1 Cu1 89.788(16) 5_655 5_656 ?
Cu2 I1 Cu1 163.501(15) . 5_656 ?
Cu3 I1 Cu1 70.853(10) . 5_656 ?
Cu1 I1 Cu1 102.65(2) . 5_656 ?
N1 Cu1 N1 157.51(17) . 2_656 ?
N1 Cu1 I1 96.46(9) . . ?
N1 Cu1 I1 101.07(9) 2_656 . ?
N1 Cu1 I1 101.07(9) . 5_656 ?
N1 Cu1 I1 96.46(9) 2_656 5_656 ?
I1 Cu1 I1 77.35(2) . 5_656 ?
N4 Cu2 N4 119.40(16) 7_656 8_454 ?
N4 Cu2 I1 107.61(8) 7_656 5_655 ?
N4 Cu2 I1 108.63(8) 8_454 5_655 ?
N4 Cu2 I1 108.63(8) 7_656 . ?
N4 Cu2 I1 107.61(8) 8_454 . ?
I1 Cu2 I1 103.89(2) 5_655 . ?
N2 Cu3 N2 149.01(16) 5_656 2_656 ?
N2 Cu3 I1 105.49(8) 5_656 . ?
N2 Cu3 I1 105.49(8) 2_656 . ?
C1 N1 N2 105.4(3) . . ?
C1 N1 Cu1 132.5(2) . . ?
N2 N1 Cu1 121.9(2) . . ?
N3 N2 N1 110.1(3) . . ?
N3 N2 Cu3 127.3(2) . 5_656 ?
N1 N2 Cu3 121.9(2) . 5_656 ?
N2 N3 N4 107.9(3) . . ?
C1 N4 N3 106.6(3) . . ?
C1 N4 Cu2 135.5(2) . 7_656 ?
N3 N4 Cu2 117.3(2) . 7_656 ?
N1 C1 N4 110.0(3) . . ?
N1 C1 C2 124.4(3) . . ?
N4 C1 C2 125.6(3) . . ?
C3 C2 C4 119.9(3) . . ?
C3 C2 C1 119.7(3) . . ?
C4 C2 C1 120.5(3) . . ?
C2 C3 C2 120.2(4) . 6_565 ?
C2 C3 H5A 119.9 . . ?
C2 C3 H5A 119.9 6_565 . ?
C2 C4 C5 120.0(3) . . ?
C2 C4 H3A 120.0 . . ?
C5 C4 H3A 120.0 . . ?
C4 C5 C4 120.1(5) 6_565 . ?
C4 C5 H4A 120.0 6_565 . ?
C4 C5 H4A 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_180k
_database_code_depnum_ccdc_archive 'CCDC 1813318'
_audit_update_record             
;
2017-12-24 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H4 Cu3 I N8'
_chemical_formula_sum            'C8 H4 Cu3 I N8'
_chemical_formula_weight         529.74

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   C2/m
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   13.716(2)
_cell_length_b                   12.690(2)
_cell_length_c                   8.0424(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.674(2)
_cell_angle_gamma                90.00
_cell_volume                     1137.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    3509
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      25.09

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.094
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    8.273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4079
_exptl_absorpt_correction_T_max  0.5484
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      180(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 Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3509
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.09
_reflns_number_total             1043
_reflns_number_gt                1001
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0326P)²+2.2796P] 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         1043
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0188
_refine_ls_wR_factor_ref         0.0548
_refine_ls_wR_factor_gt          0.0541
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.157
_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 0.52180(3) 0.5000 0.28591(4) 0.01347(13) Uani 1 2 d S . .
Cu1 Cu 0.5000 0.31118(5) 0.5000 0.02366(18) Uani 1 2 d S . .
Cu2 Cu 0.5000 0.36810(5) 0.0000 0.01873(17) Uani 1 2 d S . .
Cu3 Cu 0.29558(6) 0.5000 0.20090(10) 0.02140(18) Uani 1 2 d S . .
N1 N 0.6670(3) 0.2820(2) 0.6816(4) 0.0153(6) Uani 1 1 d . . .
N2 N 0.7470(3) 0.3542(2) 0.8162(4) 0.0150(6) Uani 1 1 d . . .
N3 N 0.8535(3) 0.3126(2) 0.9316(4) 0.0166(6) Uani 1 1 d . . .
N4 N 0.8459(3) 0.2121(2) 0.8734(4) 0.0150(6) Uani 1 1 d . . .
C1 C 0.7308(3) 0.1949(3) 0.7197(5) 0.0132(7) Uani 1 1 d . . .
C2 C 0.6807(3) 0.0951(3) 0.6085(5) 0.0150(7) Uani 1 1 d . . .
C3 C 0.7257(4) 0.0000 0.7124(7) 0.0143(9) Uani 1 2 d S . .
H5A H 0.7863 0.0000 0.8522 0.017 Uiso 1 2 calc SR . .
C4 C 0.5901(3) 0.0946(3) 0.3989(5) 0.0174(7) Uani 1 1 d . . .
H3A H 0.5596 0.1579 0.3283 0.021 Uiso 1 1 calc R . .
C5 C 0.5456(5) 0.0000 0.2958(7) 0.0203(11) Uani 1 2 d S . .
H4A H 0.4852 0.0000 0.1559 0.024 Uiso 1 2 calc SR . .

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
I1 0.0145(2) 0.01189(18) 0.01600(18) 0.000 0.00999(15) 0.000
Cu1 0.0115(3) 0.0173(3) 0.0304(4) 0.000 0.0056(3) 0.000
Cu2 0.0117(3) 0.0142(3) 0.0255(3) 0.000 0.0081(3) 0.000
Cu3 0.0255(4) 0.0072(3) 0.0315(4) 0.000 0.0166(3) 0.000
N1 0.0134(15) 0.0087(13) 0.0204(14) 0.0000(11) 0.0079(13) -0.0004(11)
N2 0.0131(16) 0.0081(13) 0.0225(14) 0.0005(11) 0.0096(13) 0.0004(11)
N3 0.0155(16) 0.0104(14) 0.0202(14) 0.0000(11) 0.0083(13) 0.0003(12)
N4 0.0158(16) 0.0096(14) 0.0174(14) -0.0008(11) 0.0085(13) -0.0010(12)
C1 0.0140(17) 0.0101(16) 0.0178(16) 0.0034(12) 0.0106(15) 0.0013(13)
C2 0.0134(17) 0.0132(17) 0.0200(16) -0.0008(13) 0.0108(15) -0.0007(13)
C3 0.011(2) 0.013(2) 0.015(2) 0.000 0.006(2) 0.000
C4 0.0192(19) 0.0128(17) 0.0196(17) 0.0044(13) 0.0109(15) 0.0029(14)
C5 0.021(3) 0.020(3) 0.018(2) 0.000 0.011(2) 0.000

_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 2.7159(5) . ?
I1 Cu2 2.7159(5) 5_665 ?
I1 Cu3 2.7607(9) . ?
I1 Cu1 3.0652(6) 5_666 ?
I1 Cu1 3.0652(6) . ?
Cu1 N1 1.902(3) 2_656 ?
Cu1 N1 1.902(3) . ?
Cu1 I1 3.0652(6) 5_666 ?
Cu2 N4 2.007(3) 8_454 ?
Cu2 N4 2.007(3) 7_656 ?
Cu2 I1 2.7159(5) 5_665 ?
Cu3 N2 1.920(3) 2_656 ?
Cu3 N2 1.920(3) 5_666 ?
N1 C1 1.330(4) . ?
N1 N2 1.353(4) . ?
N2 N3 1.301(4) . ?
N2 Cu3 1.920(3) 5_666 ?
N3 N4 1.342(4) . ?
N4 C1 1.338(5) . ?
N4 Cu2 2.007(3) 7_656 ?
C1 C2 1.469(5) . ?
C2 C3 1.391(4) . ?
C2 C4 1.394(5) . ?
C3 C2 1.391(4) 6 ?
C3 H5A 0.9300 . ?
C4 C5 1.382(4) . ?
C4 H3A 0.9300 . ?
C5 C4 1.382(4) 6 ?
C5 H4A 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
Cu2 I1 Cu2 76.09(3) . 5_665 ?
Cu2 I1 Cu3 103.734(13) . . ?
Cu2 I1 Cu3 103.734(13) 5_665 . ?
Cu2 I1 Cu1 163.471(14) . 5_666 ?
Cu2 I1 Cu1 89.724(18) 5_665 5_666 ?
Cu3 I1 Cu1 71.055(10) . 5_666 ?
Cu2 I1 Cu1 89.724(18) . . ?
Cu2 I1 Cu1 163.471(14) 5_665 . ?
Cu3 I1 Cu1 71.055(10) . . ?
Cu1 I1 Cu1 102.83(2) 5_666 . ?
N1 Cu1 N1 157.56(17) 2_656 . ?
N1 Cu1 I1 96.60(8) 2_656 5_666 ?
N1 Cu1 I1 100.91(8) . 5_666 ?
N1 Cu1 I1 100.91(8) 2_656 . ?
N1 Cu1 I1 96.60(8) . . ?
I1 Cu1 I1 77.17(2) 5_666 . ?
N4 Cu2 N4 119.10(16) 8_454 7_656 ?
N4 Cu2 I1 107.78(8) 8_454 . ?
N4 Cu2 I1 108.62(8) 7_656 . ?
N4 Cu2 I1 108.62(8) 8_454 5_665 ?
N4 Cu2 I1 107.78(8) 7_656 5_665 ?
I1 Cu2 I1 103.91(3) . 5_665 ?
N2 Cu3 N2 148.85(17) 2_656 5_666 ?
N2 Cu3 I1 105.57(9) 2_656 . ?
N2 Cu3 I1 105.57(9) 5_666 . ?
C1 N1 N2 105.2(3) . . ?
C1 N1 Cu1 132.4(2) . . ?
N2 N1 Cu1 122.3(2) . . ?
N3 N2 N1 110.2(3) . . ?
N3 N2 Cu3 127.6(2) . 5_666 ?
N1 N2 Cu3 121.6(2) . 5_666 ?
N2 N3 N4 108.1(3) . . ?
C1 N4 N3 106.7(3) . . ?
C1 N4 Cu2 135.4(2) . 7_656 ?
N3 N4 Cu2 117.4(2) . 7_656 ?
N1 C1 N4 109.9(3) . . ?
N1 C1 C2 124.4(3) . . ?
N4 C1 C2 125.7(3) . . ?
C3 C2 C4 119.5(3) . . ?
C3 C2 C1 119.7(3) . . ?
C4 C2 C1 120.7(3) . . ?
C2 C3 C2 120.4(4) 6 . ?
C2 C3 H5A 119.8 6 . ?
C2 C3 H5A 119.8 . . ?
C5 C4 C2 120.0(3) . . ?
C5 C4 H3A 120.0 . . ?
C2 C4 H3A 120.0 . . ?
C4 C5 C4 120.6(5) . 6 ?
C4 C5 H4A 119.7 . . ?
C4 C5 H4A 119.7 6 . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.121
