# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_CuL-Me2
_database_code_depnum_ccdc_archive 'CCDC 1048600'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H24 Cu N6 O 2+,2(N O3 1-)'
_chemical_formula_sum            'C16 H24 Cu N8 O7'
_chemical_formula_weight         503.97

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   6.7015(3)
_cell_length_b                   18.7764(8)
_cell_length_c                   8.4556(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.755(5)
_cell_angle_gamma                90.00
_cell_volume                     1041.65(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1786
_cell_measurement_theta_min      3.0986
_cell_measurement_theta_max      29.3644

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.2325
_exptl_crystal_size_mid          0.2103
_exptl_crystal_size_min          0.1020
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             522
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80002
_exptl_absorpt_correction_T_max  1.00000
_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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4098
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4391
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2951
_reflns_number_gt                2658
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0536P)²+0.1757P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_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   -0.034(16)
_refine_ls_number_reflns         2951
_refine_ls_number_parameters     289
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0908
_refine_ls_wR_factor_gt          0.0868
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.29766(6) -0.36974(4) 0.16263(5) 0.02835(15) Uani 1 1 d . . .
N1 N -0.4770(7) -0.4574(3) 0.1311(6) 0.0290(11) Uani 1 1 d . . .
N2 N -0.6756(7) -0.5515(3) 0.1139(6) 0.0390(13) Uani 1 1 d . . .
H2A H -0.7855 -0.5795 0.0817 0.047 Uiso 1 1 d R . .
N3 N -0.1179(6) -0.4342(2) 0.3158(5) 0.0279(10) Uani 1 1 d . . .
N4 N -0.0896(6) -0.3014(2) 0.2679(5) 0.0258(10) Uani 1 1 d . . .
N5 N -0.4653(7) -0.2792(3) 0.1214(6) 0.0293(11) Uani 1 1 d . . .
N6 N -0.6619(7) -0.1848(2) 0.1010(6) 0.0293(11) Uani 1 1 d . . .
H6B H -0.7735 -0.1571 0.0763 0.035 Uiso 1 1 d R . .
N7 N -0.9078(7) -0.0379(3) -0.7737(7) 0.0393(13) Uani 1 1 d . . .
N8 N -0.0691(7) -0.2044(3) -0.2294(8) 0.0449(14) Uani 1 1 d . . .
O1W O -0.1574(5) -0.3734(3) -0.0515(3) 0.0608(8) Uani 1 1 d . . .
H1WB H -0.1804 -0.3361 -0.1092 0.073 Uiso 1 1 d R . .
H1WA H -0.1904 -0.4104 -0.1089 0.073 Uiso 1 1 d R . .
O1 O -0.9214(9) 0.0245(3) -0.7320(6) 0.0698(15) Uani 1 1 d . . .
O2 O -0.9007(8) -0.0872(2) -0.6741(7) 0.0637(14) Uani 1 1 d . . .
O3 O -0.9004(7) -0.0517(3) -0.9162(6) 0.0642(15) Uani 1 1 d . . .
O5 O -0.0650(9) -0.1595(3) -0.3338(9) 0.092(2) Uani 1 1 d . . .
O6 O -0.0567(9) -0.2672(3) -0.2617(7) 0.0725(16) Uani 1 1 d . . .
O7 O -0.0839(8) -0.1876(3) -0.0923(6) 0.0778(18) Uani 1 1 d . . .
C1 C -0.4326(9) -0.0918(3) 0.2649(8) 0.0445(16) Uani 1 1 d . . .
H1A H -0.2926 -0.0894 0.3200 0.067 Uiso 1 1 d R . .
H1B H -0.4586 -0.0557 0.1829 0.067 Uiso 1 1 d R . .
H1C H -0.5193 -0.0842 0.3408 0.067 Uiso 1 1 d R . .
C2 C -0.4761(9) -0.1642(3) 0.1928(8) 0.0326(14) Uani 1 1 d . . .
C3 C -0.6502(9) -0.2535(3) 0.0604(7) 0.0329(15) Uani 1 1 d . . .
H3A H -0.7595 -0.2798 -0.0052 0.040 Uiso 1 1 d R . .
C4 C -0.3569(9) -0.2229(3) 0.2034(7) 0.0281(13) Uani 1 1 d . . .
C5 C -0.1472(8) -0.2376(3) 0.2824(7) 0.0315(13) Uani 1 1 d . . .
H5A H -0.0604 -0.2020 0.3425 0.038 Uiso 1 1 d R . .
C6 C 0.1056(6) -0.3330(2) 0.3415(5) 0.0274(9) Uani 1 1 d . . .
H6A H 0.1712 -0.3482 0.2564 0.033 Uiso 1 1 d R . .
C7 C 0.2565(8) -0.2878(3) 0.4560(7) 0.0328(14) Uani 1 1 d . . .
H7A H 0.1958 -0.2724 0.5438 0.039 Uiso 1 1 d R . .
H7B H 0.2918 -0.2463 0.4011 0.039 Uiso 1 1 d R . .
C8 C 0.4480(7) -0.3326(3) 0.5238(7) 0.0439(12) Uani 1 1 d . . .
H8A H 0.5413 -0.3048 0.6010 0.053 Uiso 1 1 d R . .
H8B H 0.5140 -0.3442 0.4364 0.053 Uiso 1 1 d R . .
C9 C 0.3989(7) -0.4012(3) 0.6027(7) 0.0496(14) Uani 1 1 d . . .
H9A H 0.3462 -0.3896 0.6969 0.059 Uiso 1 1 d R . .
H9B H 0.5210 -0.4287 0.6367 0.059 Uiso 1 1 d R . .
C10 C 0.2400(8) -0.4456(3) 0.4865(8) 0.0373(15) Uani 1 1 d . . .
H10A H 0.2030 -0.4866 0.5417 0.045 Uiso 1 1 d R . .
H10B H 0.2965 -0.4615 0.3971 0.045 Uiso 1 1 d R . .
C11 C 0.0521(6) -0.4002(2) 0.4264(5) 0.0278(9) Uani 1 1 d . . .
H11A H 0.0014 -0.3846 0.5189 0.033 Uiso 1 1 d R . .
C12 C -0.1777(8) -0.4978(3) 0.3230(7) 0.0303(13) Uani 1 1 d . . .
H12A H -0.0988 -0.5327 0.3918 0.036 Uiso 1 1 d R . .
C13 C -0.3745(9) -0.5135(3) 0.2236(7) 0.0301(13) Uani 1 1 d . . .
C14 C -0.6579(9) -0.4833(3) 0.0689(7) 0.0354(15) Uani 1 1 d . . .
H14A H -0.7648 -0.4564 0.0022 0.042 Uiso 1 1 d R . .
C15 C -0.4970(9) -0.5722(3) 0.2116(7) 0.0303(13) Uani 1 1 d . . .
C16 C -0.4621(9) -0.6433(3) 0.2875(8) 0.0431(15) Uani 1 1 d . . .
H16A H -0.3269 -0.6461 0.3523 0.065 Uiso 1 1 d R . .
H16B H -0.5598 -0.6514 0.3543 0.065 Uiso 1 1 d R . .
H16C H -0.4782 -0.6789 0.2043 0.065 Uiso 1 1 d 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
Cu1 N4 1.969(4) . ?
Cu1 N3 1.990(4) . ?
Cu1 N1 2.023(5) . ?
Cu1 N5 2.029(5) . ?
Cu1 O1W 2.204(3) . ?
N1 C14 1.313(8) . ?
N1 C13 1.406(8) . ?
N2 C14 1.348(8) . ?
N2 C15 1.365(8) . ?
N3 C12 1.265(6) . ?
N3 C11 1.465(6) . ?
N4 C5 1.273(7) . ?
N4 C6 1.456(6) . ?
N5 C3 1.331(8) . ?
N5 C4 1.385(7) . ?
N6 C3 1.341(7) . ?
N6 C2 1.382(8) . ?
N7 O1 1.232(7) . ?
N7 O3 1.243(7) . ?
N7 O2 1.246(7) . ?
N8 O5 1.225(7) . ?
N8 O7 1.224(7) . ?
N8 O6 1.217(7) . ?
C1 C2 1.493(8) . ?
C2 C4 1.355(8) . ?
C4 C5 1.454(8) . ?
C6 C7 1.511(7) . ?
C6 C11 1.530(5) . ?
C7 C8 1.544(7) . ?
C8 C9 1.518(6) . ?
C9 C10 1.539(8) . ?
C10 C11 1.519(7) . ?
C12 C13 1.442(9) . ?
C13 C15 1.365(8) . ?
C15 C16 1.480(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N3 79.82(13) . . ?
N4 Cu1 N1 159.49(18) . . ?
N3 Cu1 N1 81.7(2) . . ?
N4 Cu1 N5 81.25(19) . . ?
N3 Cu1 N5 149.61(18) . . ?
N1 Cu1 N5 111.45(11) . . ?
N4 Cu1 O1W 90.61(16) . . ?
N3 Cu1 O1W 102.27(16) . . ?
N1 Cu1 O1W 101.97(18) . . ?
N5 Cu1 O1W 101.48(19) . . ?
C14 N1 C13 104.5(5) . . ?
C14 N1 Cu1 146.1(5) . . ?
C13 N1 Cu1 109.1(4) . . ?
C14 N2 C15 108.9(5) . . ?
C12 N3 C11 126.4(5) . . ?
C12 N3 Cu1 116.7(4) . . ?
C11 N3 Cu1 116.0(3) . . ?
C5 N4 C6 127.4(5) . . ?
C5 N4 Cu1 117.1(4) . . ?
C6 N4 Cu1 114.8(3) . . ?
C3 N5 C4 105.7(5) . . ?
C3 N5 Cu1 144.0(5) . . ?
C4 N5 Cu1 109.7(4) . . ?
C3 N6 C2 108.7(5) . . ?
O1 N7 O3 119.7(6) . . ?
O1 N7 O2 120.5(6) . . ?
O3 N7 O2 119.8(6) . . ?
O5 N8 O7 121.5(8) . . ?
O5 N8 O6 119.5(7) . . ?
O7 N8 O6 118.9(7) . . ?
C4 C2 N6 105.1(5) . . ?
C4 C2 C1 130.6(6) . . ?
N6 C2 C1 124.3(5) . . ?
N5 C3 N6 110.3(6) . . ?
C2 C4 N5 110.2(5) . . ?
C2 C4 C5 133.3(5) . . ?
N5 C4 C5 116.4(5) . . ?
N4 C5 C4 114.7(5) . . ?
N4 C6 C7 118.1(4) . . ?
N4 C6 C11 105.1(3) . . ?
C7 C6 C11 110.7(4) . . ?
C6 C7 C8 109.2(4) . . ?
C9 C8 C7 112.8(4) . . ?
C10 C9 C8 111.3(5) . . ?
C9 C10 C11 109.2(5) . . ?
N3 C11 C6 106.6(3) . . ?
N3 C11 C10 116.9(4) . . ?
C6 C11 C10 111.2(4) . . ?
N3 C12 C13 115.2(5) . . ?
C15 C13 N1 110.2(5) . . ?
C15 C13 C12 132.3(6) . . ?
N1 C13 C12 117.2(5) . . ?
N1 C14 N2 111.5(6) . . ?
C13 C15 N2 104.8(5) . . ?
C13 C15 C16 131.0(6) . . ?
N2 C15 C16 124.1(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.066
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1048601'
_audit_update_record             
;
2015-02-09 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H16 Cu2 Ni I2 N6, C3 H7 N O'
_chemical_formula_sum            'C17 H23 Cu2 I2 N7 Ni O'
_chemical_formula_weight         781.01

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'
Ni Ni 0.3393 1.1124 '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           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7755(9)
_cell_length_b                   11.4427(6)
_cell_length_c                   12.7640(8)
_cell_angle_alpha                82.939(5)
_cell_angle_beta                 70.893(7)
_cell_angle_gamma                88.924(6)
_cell_volume                     1201.59(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2020
_cell_measurement_theta_min      3.5880
_cell_measurement_theta_max      21.7000

_exptl_crystal_description       cuboid
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.1693
_exptl_crystal_size_mid          0.0803
_exptl_crystal_size_min          0.0565
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             748
_exptl_absorpt_coefficient_mu    5.121
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_T_max  0.679
_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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4471
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10031
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0877
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         25.35
_reflns_number_total             4390
_reflns_number_gt                2645
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0398P)²+1.8988P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4390
_refine_ls_number_parameters     290
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1401
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.084
_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 0.65187(12) 0.66312(7) -0.03944(7) 0.0794(3) Uani 1 1 d . . .
I2 I 0.87933(11) 1.02444(7) 0.36902(7) 0.0740(3) Uani 1 1 d . . .
Cu1 Cu 0.5318(2) 0.47937(13) 0.09138(11) 0.0658(4) Uani 1 1 d . . .
Cu2 Cu 0.96854(18) 0.89280(11) 0.51405(12) 0.0649(4) Uani 1 1 d . . .
Ni1 Ni 0.69667(16) 0.41035(9) 0.52066(9) 0.0394(3) Uani 1 1 d . A .
O1 O -0.1357(15) 0.7089(10) 0.2090(10) 0.135(4) Uani 1 1 d DU . .
N1 N 0.5640(11) 0.4225(7) 0.2314(7) 0.053(2) Uani 1 1 d . . .
N2 N 0.6329(10) 0.4143(6) 0.3875(6) 0.046(2) Uani 1 1 d . A .
N3 N 0.5884(11) 0.2558(6) 0.5571(7) 0.054(2) Uani 1 1 d D . .
N4 N 0.7330(12) 0.3599(7) 0.6614(7) 0.058(3) Uani 1 1 d D . .
N5 N 0.8044(10) 0.5548(6) 0.5306(6) 0.045(2) Uani 1 1 d . . .
N6 N 0.9130(11) 0.7248(7) 0.5403(7) 0.057(2) Uani 1 1 d . . .
N7 N 0.0161(14) 0.7517(11) 0.0294(11) 0.096(4) Uani 1 1 d DU . .
C1 C 0.6356(13) 0.4790(9) 0.2926(8) 0.050(3) Uani 1 1 d . . .
H1 H 0.6811 0.5544 0.2702 0.061 Uiso 1 1 calc R . .
C2 C 0.5120(14) 0.3175(8) 0.2945(8) 0.052(3) Uani 1 1 d . A .
H2 H 0.4571 0.2594 0.2753 0.063 Uiso 1 1 calc R . .
C3 C 0.5510(12) 0.3092(7) 0.3891(8) 0.042(2) Uani 1 1 d . . .
C4 C 0.5337(14) 0.2243(9) 0.4830(9) 0.058(3) Uani 1 1 d . A .
H4 H 0.4858 0.1505 0.4904 0.069 Uiso 1 1 calc R . .
C5 C 0.635(3) 0.1722(12) 0.6379(11) 0.041(5) Uani 0.50 1 d PD A 1
H5 H 0.7443 0.1455 0.6018 0.050 Uiso 0.50 1 calc PR A 1
C6 C 0.524(3) 0.0641(15) 0.6977(19) 0.057(3) Uani 0.50 1 d PD A 1
H6A H 0.4163 0.0895 0.7352 0.068 Uiso 0.50 1 calc PR A 1
H6B H 0.5188 0.0134 0.6434 0.068 Uiso 0.50 1 calc PR A 1
C7 C 0.593(3) -0.0040(11) 0.7834(16) 0.061(6) Uani 0.50 1 d PD A 1
H7A H 0.6990 -0.0323 0.7451 0.073 Uiso 0.50 1 calc PR A 1
H7B H 0.5234 -0.0717 0.8218 0.073 Uiso 0.50 1 calc PR A 1
C8 C 0.605(3) 0.0762(16) 0.8690(13) 0.063(8) Uani 0.50 1 d PD A 1
H8A H 0.4981 0.1013 0.9100 0.076 Uiso 0.50 1 calc PR A 1
H8B H 0.6494 0.0327 0.9220 0.076 Uiso 0.50 1 calc PR A 1
C9 C 0.713(3) 0.1846(19) 0.809(2) 0.064(3) Uani 0.50 1 d PD A 1
H9A H 0.8210 0.1600 0.7693 0.076 Uiso 0.50 1 calc PR A 1
H9B H 0.7207 0.2350 0.8629 0.076 Uiso 0.50 1 calc PR A 1
C10 C 0.639(3) 0.2528(10) 0.7254(15) 0.063(9) Uani 0.50 1 d PD A 1
H10 H 0.5292 0.2746 0.7659 0.075 Uiso 0.50 1 calc PR A 1
C5' C 0.564(3) 0.2077(12) 0.6741(10) 0.041(5) Uani 0.50 1 d PD A 2
H5' H 0.4769 0.2498 0.7238 0.050 Uiso 0.50 1 calc PR A 2
C6' C 0.523(3) 0.0749(15) 0.6974(19) 0.057(3) Uani 0.50 1 d PD A 2
H6'A H 0.4212 0.0606 0.6860 0.068 Uiso 0.50 1 calc PR A 2
H6'B H 0.6060 0.0333 0.6458 0.068 Uiso 0.50 1 calc PR A 2
C7' C 0.511(2) 0.0287(15) 0.8180(17) 0.061(6) Uani 0.50 1 d PD A 2
H7'A H 0.4888 -0.0556 0.8312 0.073 Uiso 0.50 1 calc PR A 2
H7'B H 0.4223 0.0660 0.8694 0.073 Uiso 0.50 1 calc PR A 2
C8' C 0.669(3) 0.0541(16) 0.8397(17) 0.063(8) Uani 0.50 1 d PD A 2
H8'A H 0.6576 0.0263 0.9168 0.076 Uiso 0.50 1 calc PR A 2
H8'B H 0.7560 0.0123 0.7919 0.076 Uiso 0.50 1 calc PR A 2
C9' C 0.708(3) 0.1869(18) 0.816(2) 0.064(3) Uani 0.50 1 d PD A 2
H9'A H 0.8086 0.2021 0.8290 0.076 Uiso 0.50 1 calc PR A 2
H9'B H 0.6233 0.2286 0.8665 0.076 Uiso 0.50 1 calc PR A 2
C10' C 0.723(3) 0.2309(10) 0.6944(18) 0.063(9) Uani 0.50 1 d PD A 2
H10' H 0.8121 0.1923 0.6428 0.075 Uiso 0.50 1 calc PR A 2
C11 C 0.8071(14) 0.4319(9) 0.6968(8) 0.057(3) Uani 1 1 d . A .
H11 H 0.8346 0.4140 0.7613 0.069 Uiso 1 1 calc R . .
C12 C 0.8449(13) 0.5451(8) 0.6273(8) 0.050(3) Uani 1 1 d . A .
C13 C 0.9143(14) 0.6493(9) 0.6306(9) 0.055(3) Uani 1 1 d . A .
H13 H 0.9557 0.6660 0.6857 0.066 Uiso 1 1 calc R . .
C14 C 0.8460(13) 0.6654(8) 0.4829(8) 0.050(3) Uani 1 1 d . A .
H14 H 0.8298 0.6973 0.4168 0.059 Uiso 1 1 calc R . .
C15 C -0.0902(17) 0.7838(15) 0.1240(12) 0.159(8) Uani 1 1 d DU . .
H15 H -0.1289 0.8600 0.1261 0.191 Uiso 1 1 calc R . .
C16 C 0.077(3) 0.6348(16) 0.025(2) 0.231(13) Uani 1 1 d DU . .
H16A H 0.0319 0.5892 0.0964 0.347 Uiso 1 1 calc R . .
H16B H 0.1922 0.6380 0.0043 0.347 Uiso 1 1 calc R . .
H16C H 0.0470 0.5988 -0.0302 0.347 Uiso 1 1 calc R . .
C17 C 0.067(3) 0.838(2) -0.0675(19) 0.293(17) Uani 1 1 d DU . .
H17A H -0.0153 0.8460 -0.1019 0.440 Uiso 1 1 calc R . .
H17B H 0.1649 0.8132 -0.1196 0.440 Uiso 1 1 calc R . .
H17C H 0.0861 0.9123 -0.0457 0.440 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 Cu1 2.5273(16) . ?
I1 Cu1 2.6002(16) 2_665 ?
I2 Cu2 2.5549(18) . ?
I2 Cu2 2.5701(16) 2_776 ?
Cu1 N1 1.933(8) . ?
Cu1 Cu1 2.559(3) 2_665 ?
Cu1 I1 2.6002(16) 2_665 ?
Cu2 N6 1.953(8) . ?
Cu2 Cu2 2.481(2) 2_776 ?
Cu2 I2 2.5701(16) 2_776 ?
Ni1 N4 1.943(8) . ?
Ni1 N2 1.951(8) . ?
Ni1 N3 1.954(7) . ?
Ni1 N5 1.957(7) . ?
O1 C15 1.254(9) . ?
N1 C2 1.357(12) . ?
N1 C1 1.372(12) . ?
N2 C1 1.333(12) . ?
N2 C3 1.407(11) . ?
N3 C4 1.282(12) . ?
N3 C5 1.470(12) . ?
N3 C5' 1.472(11) . ?
N4 C11 1.269(11) . ?
N4 C10' 1.481(13) . ?
N4 C10 1.482(13) . ?
N5 C14 1.337(11) . ?
N5 C12 1.384(12) . ?
N6 C14 1.327(11) . ?
N6 C13 1.356(13) . ?
N7 C15 1.350(9) . ?
N7 C16 1.431(10) . ?
N7 C17 1.434(10) . ?
C1 H1 0.9300 . ?
C2 C3 1.351(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.415(13) . ?
C4 H4 0.9300 . ?
C5 C10 1.543(10) . ?
C5 C6 1.544(10) . ?
C5 H5 0.9800 . ?
C6 C7 1.539(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.540(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.538(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.546(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10 0.9800 . ?
C5' C10' 1.537(10) . ?
C5' C6' 1.538(9) . ?
C5' H5' 0.9800 . ?
C6' C7' 1.535(10) . ?
C6' H6'A 0.9700 . ?
C6' H6'B 0.9700 . ?
C7' C8' 1.536(10) . ?
C7' H7'A 0.9700 . ?
C7' H7'B 0.9700 . ?
C8' C9' 1.535(10) . ?
C8' H8'A 0.9700 . ?
C8' H8'B 0.9700 . ?
C9' C10' 1.539(10) . ?
C9' H9'A 0.9700 . ?
C9' H9'B 0.9700 . ?
C10' H10' 0.9800 . ?
C11 C12 1.454(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.361(13) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cu1 I1 Cu1 59.86(5) . 2_665 ?
Cu2 I2 Cu2 57.91(5) . 2_776 ?
N1 Cu1 I1 127.9(3) . . ?
N1 Cu1 Cu1 170.4(3) . 2_665 ?
I1 Cu1 Cu1 61.48(6) . 2_665 ?
N1 Cu1 I1 111.9(2) . 2_665 ?
I1 Cu1 I1 120.14(5) . 2_665 ?
Cu1 Cu1 I1 58.66(6) 2_665 2_665 ?
N6 Cu2 Cu2 178.2(3) . 2_776 ?
N6 Cu2 I2 118.9(3) . . ?
Cu2 Cu2 I2 61.35(6) 2_776 . ?
N6 Cu2 I2 119.0(3) . 2_776 ?
Cu2 Cu2 I2 60.74(6) 2_776 2_776 ?
I2 Cu2 I2 122.09(5) . 2_776 ?
N4 Ni1 N2 163.1(3) . . ?
N4 Ni1 N3 80.6(3) . . ?
N2 Ni1 N3 82.5(3) . . ?
N4 Ni1 N5 82.5(3) . . ?
N2 Ni1 N5 114.5(3) . . ?
N3 Ni1 N5 162.7(3) . . ?
C2 N1 C1 104.2(8) . . ?
C2 N1 Cu1 126.8(7) . . ?
C1 N1 Cu1 129.0(7) . . ?
C1 N2 C3 104.7(7) . . ?
C1 N2 Ni1 144.5(6) . . ?
C3 N2 Ni1 110.8(6) . . ?
C4 N3 C5 123.7(10) . . ?
C4 N3 C5' 132.4(11) . . ?
C5 N3 C5' 31.0(9) . . ?
C4 N3 Ni1 115.6(7) . . ?
C5 N3 Ni1 115.7(9) . . ?
C5' N3 Ni1 111.1(8) . . ?
C11 N4 C10' 124.6(12) . . ?
C11 N4 C10 127.1(11) . . ?
C10' N4 C10 29.9(14) . . ?
C11 N4 Ni1 117.0(7) . . ?
C10' N4 Ni1 114.9(10) . . ?
C10 N4 Ni1 114.4(9) . . ?
C14 N5 C12 104.9(7) . . ?
C14 N5 Ni1 144.0(7) . . ?
C12 N5 Ni1 110.8(6) . . ?
C14 N6 C13 106.1(8) . . ?
C14 N6 Cu2 127.3(8) . . ?
C13 N6 Cu2 126.0(6) . . ?
C15 N7 C16 121.4(17) . . ?
C15 N7 C17 118.3(18) . . ?
C16 N7 C17 120(2) . . ?
N2 C1 N1 112.9(8) . . ?
N2 C1 H1 123.5 . . ?
N1 C1 H1 123.5 . . ?
C3 C2 N1 110.6(8) . . ?
C3 C2 H2 124.7 . . ?
N1 C2 H2 124.7 . . ?
C2 C3 N2 107.5(8) . . ?
C2 C3 C4 137.0(9) . . ?
N2 C3 C4 115.5(8) . . ?
N3 C4 C3 115.5(9) . . ?
N3 C4 H4 122.2 . . ?
C3 C4 H4 122.2 . . ?
N3 C5 C10 101.2(12) . . ?
N3 C5 C6 119.2(15) . . ?
C10 C5 C6 108.9(9) . . ?
N3 C5 H5 109.0 . . ?
C10 C5 H5 109.0 . . ?
C6 C5 H5 109.0 . . ?
C7 C6 C5 109.2(9) . . ?
C7 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
C7 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
C6 C7 C8 110.3(9) . . ?
C6 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C7 110.1(9) . . ?
C9 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 C10 108.7(9) . . ?
C8 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
C8 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.3 . . ?
N4 C10 C5 105.9(13) . . ?
N4 C10 C9 114.2(16) . . ?
C5 C10 C9 108.9(9) . . ?
N4 C10 H10 109.2 . . ?
C5 C10 H10 109.2 . . ?
C9 C10 H10 109.2 . . ?
N3 C5' C10' 105.9(15) . . ?
N3 C5' C6' 112.7(12) . . ?
C10' C5' C6' 109.8(9) . . ?
N3 C5' H5' 109.5 . . ?
C10' C5' H5' 109.5 . . ?
C6' C5' H5' 109.5 . . ?
C7' C6' C5' 110.0(9) . . ?
C7' C6' H6'A 109.7 . . ?
C5' C6' H6'A 109.7 . . ?
C7' C6' H6'B 109.7 . . ?
C5' C6' H6'B 109.7 . . ?
H6'A C6' H6'B 108.2 . . ?
C6' C7' C8' 110.8(9) . . ?
C6' C7' H7'A 109.5 . . ?
C8' C7' H7'A 109.5 . . ?
C6' C7' H7'B 109.5 . . ?
C8' C7' H7'B 109.5 . . ?
H7'A C7' H7'B 108.1 . . ?
C9' C8' C7' 110.3(9) . . ?
C9' C8' H8'A 109.6 . . ?
C7' C8' H8'A 109.6 . . ?
C9' C8' H8'B 109.6 . . ?
C7' C8' H8'B 109.6 . . ?
H8'A C8' H8'B 108.1 . . ?
C8' C9' C10' 109.4(9) . . ?
C8' C9' H9'A 109.8 . . ?
C10' C9' H9'A 109.8 . . ?
C8' C9' H9'B 109.8 . . ?
C10' C9' H9'B 109.8 . . ?
H9'A C9' H9'B 108.2 . . ?
N4 C10' C5' 97.4(13) . . ?
N4 C10' C9' 117.3(16) . . ?
C5' C10' C9' 110.0(9) . . ?
N4 C10' H10' 110.5 . . ?
C5' C10' H10' 110.5 . . ?
C9' C10' H10' 110.5 . . ?
N4 C11 C12 113.8(9) . . ?
N4 C11 H11 123.1 . . ?
C12 C11 H11 123.1 . . ?
C13 C12 N5 107.8(8) . . ?
C13 C12 C11 136.5(9) . . ?
N5 C12 C11 115.7(8) . . ?
N6 C13 C12 108.6(9) . . ?
N6 C13 H13 125.7 . . ?
C12 C13 H13 125.7 . . ?
N6 C14 N5 112.6(9) . . ?
N6 C14 H14 123.7 . . ?
N5 C14 H14 123.7 . . ?
O1 C15 N7 118.7(17) . . ?
O1 C15 H15 120.6 . . ?
N7 C15 H15 120.6 . . ?
N7 C16 H16A 109.5 . . ?
N7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N7 C17 H17A 109.5 . . ?
N7 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N7 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 I1 Cu1 N1 177.6(4) 2_665 . . . ?
Cu1 I1 Cu1 I1 0.0 2_665 . . 2_665 ?
Cu2 I2 Cu2 N6 177.9(3) 2_776 . . . ?
Cu2 I2 Cu2 I2 0.0 2_776 . . 2_776 ?
I1 Cu1 N1 C2 -172.6(8) . . . . ?
Cu1 Cu1 N1 C2 -5(3) 2_665 . . . ?
I1 Cu1 N1 C2 5.2(10) 2_665 . . . ?
I1 Cu1 N1 C1 11.1(11) . . . . ?
Cu1 Cu1 N1 C1 178.5(13) 2_665 . . . ?
I1 Cu1 N1 C1 -171.1(8) 2_665 . . . ?
N4 Ni1 N2 C1 -176.7(13) . . . . ?
N3 Ni1 N2 C1 178.8(13) . . . . ?
N5 Ni1 N2 C1 2.1(14) . . . . ?
N4 Ni1 N2 C3 3.5(17) . . . . ?
N3 Ni1 N2 C3 -1.0(7) . . . . ?
N5 Ni1 N2 C3 -177.7(6) . . . . ?
N4 Ni1 N3 C4 -176.0(9) . . . . ?
N2 Ni1 N3 C4 2.7(9) . . . . ?
N5 Ni1 N3 C4 172.7(11) . . . . ?
N4 Ni1 N3 C5 -20.1(9) . . . . ?
N2 Ni1 N3 C5 158.6(10) . . . . ?
N5 Ni1 N3 C5 -31.4(18) . . . . ?
N4 Ni1 N3 C5' 13.4(10) . . . . ?
N2 Ni1 N3 C5' -167.9(10) . . . . ?
N5 Ni1 N3 C5' 2.0(18) . . . . ?
N2 Ni1 N4 C11 177.3(11) . . . . ?
N3 Ni1 N4 C11 -178.2(9) . . . . ?
N5 Ni1 N4 C11 -1.6(9) . . . . ?
N2 Ni1 N4 C10' 17(2) . . . . ?
N3 Ni1 N4 C10' 22.1(11) . . . . ?
N5 Ni1 N4 C10' -161.3(11) . . . . ?
N2 Ni1 N4 C10 -15.5(19) . . . . ?
N3 Ni1 N4 C10 -11.0(11) . . . . ?
N5 Ni1 N4 C10 165.6(11) . . . . ?
N4 Ni1 N5 C14 -173.9(12) . . . . ?
N2 Ni1 N5 C14 6.4(13) . . . . ?
N3 Ni1 N5 C14 -162.6(13) . . . . ?
N4 Ni1 N5 C12 -0.7(7) . . . . ?
N2 Ni1 N5 C12 179.7(7) . . . . ?
N3 Ni1 N5 C12 10.7(17) . . . . ?
Cu2 Cu2 N6 C14 104(9) 2_776 . . . ?
I2 Cu2 N6 C14 7.4(10) . . . . ?
I2 Cu2 N6 C14 -174.6(8) 2_776 . . . ?
Cu2 Cu2 N6 C13 -66(10) 2_776 . . . ?
I2 Cu2 N6 C13 -162.4(8) . . . . ?
I2 Cu2 N6 C13 15.6(10) 2_776 . . . ?
C3 N2 C1 N1 -1.2(12) . . . . ?
Ni1 N2 C1 N1 179.1(9) . . . . ?
C2 N1 C1 N2 1.2(12) . . . . ?
Cu1 N1 C1 N2 178.1(7) . . . . ?
C1 N1 C2 C3 -0.7(12) . . . . ?
Cu1 N1 C2 C3 -177.7(7) . . . . ?
N1 C2 C3 N2 0.0(13) . . . . ?
N1 C2 C3 C4 -178.4(12) . . . . ?
C1 N2 C3 C2 0.7(12) . . . . ?
Ni1 N2 C3 C2 -179.4(7) . . . . ?
C1 N2 C3 C4 179.5(9) . . . . ?
Ni1 N2 C3 C4 -0.7(11) . . . . ?
C5 N3 C4 C3 -157.6(12) . . . . ?
C5' N3 C4 C3 164.4(13) . . . . ?
Ni1 N3 C4 C3 -3.8(14) . . . . ?
C2 C3 C4 N3 -178.8(13) . . . . ?
N2 C3 C4 N3 2.9(15) . . . . ?
C4 N3 C5 C10 -163.3(13) . . . . ?
C5' N3 C5 C10 -46(2) . . . . ?
Ni1 N3 C5 C10 42.9(14) . . . . ?
C4 N3 C5 C6 -44.0(18) . . . . ?
C5' N3 C5 C6 74(3) . . . . ?
Ni1 N3 C5 C6 162.2(12) . . . . ?
N3 C5 C6 C7 -175.9(14) . . . . ?
C10 C5 C6 C7 -60.6(17) . . . . ?
C5 C6 C7 C8 58.7(18) . . . . ?
C6 C7 C8 C9 -58.6(17) . . . . ?
C7 C8 C9 C10 59.6(17) . . . . ?
C11 N4 C10 C5 -157.3(12) . . . . ?
C10' N4 C10 C5 -61(3) . . . . ?
Ni1 N4 C10 C5 37.0(16) . . . . ?
C11 N4 C10 C9 -37(2) . . . . ?
C10' N4 C10 C9 59(3) . . . . ?
Ni1 N4 C10 C9 156.8(12) . . . . ?
N3 C5 C10 N4 -47.8(17) . . . . ?
C6 C5 C10 N4 -174.3(15) . . . . ?
N3 C5 C10 C9 -171.0(16) . . . . ?
C6 C5 C10 C9 62.5(16) . . . . ?
C8 C9 C10 N4 -179.9(16) . . . . ?
C8 C9 C10 C5 -61.7(16) . . . . ?
C4 N3 C5' C10' 147.3(14) . . . . ?
C5 N3 C5' C10' 61(3) . . . . ?
Ni1 N3 C5' C10' -44.2(13) . . . . ?
C4 N3 C5' C6' 27(2) . . . . ?
C5 N3 C5' C6' -59(2) . . . . ?
Ni1 N3 C5' C6' -164.2(11) . . . . ?
N3 C5' C6' C7' 175.8(17) . . . . ?
C10' C5' C6' C7' 58.1(18) . . . . ?
C5' C6' C7' C8' -57.2(18) . . . . ?
C6' C7' C8' C9' 57.7(18) . . . . ?
C7' C8' C9' C10' -58.5(18) . . . . ?
C11 N4 C10' C5' 153.9(13) . . . . ?
C10 N4 C10' C5' 48(2) . . . . ?
Ni1 N4 C10' C5' -48.0(15) . . . . ?
C11 N4 C10' C9' 37(2) . . . . ?
C10 N4 C10' C9' -69(3) . . . . ?
Ni1 N4 C10' C9' -165.1(12) . . . . ?
N3 C5' C10' N4 55.7(16) . . . . ?
C6' C5' C10' N4 177.6(14) . . . . ?
N3 C5' C10' C9' 178.3(13) . . . . ?
C6' C5' C10' C9' -59.8(17) . . . . ?
C8' C9' C10' N4 169.8(17) . . . . ?
C8' C9' C10' C5' 59.8(17) . . . . ?
C10' N4 C11 C12 160.9(14) . . . . ?
C10 N4 C11 C12 -162.0(14) . . . . ?
Ni1 N4 C11 C12 3.3(13) . . . . ?
C14 N5 C12 C13 -2.2(12) . . . . ?
Ni1 N5 C12 C13 -178.1(7) . . . . ?
C14 N5 C12 C11 178.5(10) . . . . ?
Ni1 N5 C12 C11 2.5(12) . . . . ?
N4 C11 C12 C13 177.0(13) . . . . ?
N4 C11 C12 N5 -3.9(15) . . . . ?
C14 N6 C13 C12 -1.0(12) . . . . ?
Cu2 N6 C13 C12 170.6(8) . . . . ?
N5 C12 C13 N6 2.0(12) . . . . ?
C11 C12 C13 N6 -178.8(13) . . . . ?
C13 N6 C14 N5 -0.4(12) . . . . ?
Cu2 N6 C14 N5 -171.9(7) . . . . ?
C12 N5 C14 N6 1.6(12) . . . . ?
Ni1 N5 C14 N6 175.2(8) . . . . ?
C16 N7 C15 O1 0.1(3) . . . . ?
C17 N7 C15 O1 179.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.126
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1048602'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H32 Cu11 N21'
_chemical_formula_sum            'C37 H32 Cu11 N21'
_chemical_formula_weight         1469.78

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9826(4)
_cell_length_b                   12.5733(5)
_cell_length_c                   13.7208(5)
_cell_angle_alpha                79.779(3)
_cell_angle_beta                 83.639(4)
_cell_angle_gamma                82.562(4)
_cell_volume                     1338.41(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4972
_cell_measurement_theta_min      3.2150
_cell_measurement_theta_max      27.3930

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.1543
_exptl_crystal_size_mid          0.0783
_exptl_crystal_size_min          0.0506
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_absorpt_coefficient_mu    4.321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.47576
_exptl_absorpt_correction_T_max  1.00000
_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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4471
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14026
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         27.59
_reflns_number_total             5979
_reflns_number_gt                4676
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0832P)²+10.1609P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5979
_refine_ls_number_parameters     331
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0715
_refine_ls_wR_factor_ref         0.2223
_refine_ls_wR_factor_gt          0.2117
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.159
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.92816(14) 1.19976(8) 0.28347(8) 0.0432(3) Uani 1 1 d . . .
Cu2 Cu 1.0000 0.5000 0.5000 0.0514(4) Uani 1 2 d S . .
Cu3 Cu 0.71472(19) 0.58698(12) 0.38608(13) 0.0743(5) Uani 1 1 d . . .
Cu4 Cu 0.63196(18) 0.55553(11) 0.20111(14) 0.0737(5) Uani 1 1 d . . .
Cu5 Cu 0.14838(14) 0.83032(8) 0.24224(8) 0.0432(3) Uani 1 1 d . . .
Cu6 Cu 0.66438(13) 0.89416(8) 0.64686(7) 0.0373(3) Uani 1 1 d . A .
N1 N 0.7925(10) 1.1358(6) 0.4096(6) 0.0451(17) Uani 1 1 d . . .
N2 N 0.7124(9) 1.0081(5) 0.5359(5) 0.0377(15) Uani 1 1 d . A .
N3 N 0.5146(8) 1.0114(6) 0.6973(5) 0.0370(15) Uani 1 1 d D . .
N4 N 0.5640(10) 0.8069(6) 0.7662(5) 0.0427(17) Uani 1 1 d D . .
N5 N 0.7756(9) 0.7514(5) 0.6246(5) 0.0397(16) Uani 1 1 d . . .
N6 N 0.8911(10) 0.5929(6) 0.5839(5) 0.0454(17) Uani 1 1 d . . .
C1 C 0.8081(11) 1.0317(6) 0.4510(6) 0.0374(17) Uani 1 1 d . . .
H1 H 0.8805 0.9791 0.4227 0.045 Uiso 1 1 calc R . .
C2 C 0.6757(12) 1.1839(7) 0.4737(7) 0.047(2) Uani 1 1 d . A .
H2 H 0.6372 1.2577 0.4658 0.056 Uiso 1 1 calc R . .
C3 C 0.6238(11) 1.1071(7) 0.5513(6) 0.0393(18) Uani 1 1 d . . .
C4 C 0.5130(10) 1.1039(7) 0.6418(6) 0.0377(17) Uani 1 1 d . A .
H4 H 0.4451 1.1651 0.6585 0.045 Uiso 1 1 calc R . .
C5 C 0.4543(18) 0.9825(12) 0.8022(8) 0.038(4) Uani 0.50 1 d PDU A 1
H5 H 0.5482 0.9836 0.8422 0.045 Uiso 0.50 1 calc PR A 1
C6 C 0.299(2) 1.0527(10) 0.8427(12) 0.042(4) Uani 0.50 1 d PDU A 1
H6A H 0.2039 1.0521 0.8046 0.050 Uiso 0.50 1 calc PR A 1
H6B H 0.3242 1.1272 0.8358 0.050 Uiso 0.50 1 calc PR A 1
C7 C 0.252(2) 1.0084(13) 0.9529(11) 0.047(4) Uani 0.50 1 d PDU A 1
H7A H 0.3441 1.0139 0.9916 0.057 Uiso 0.50 1 calc PR A 1
H7B H 0.1519 1.0519 0.9773 0.057 Uiso 0.50 1 calc PR A 1
C8 C 0.217(2) 0.8892(13) 0.9663(11) 0.050(4) Uani 0.50 1 d PDU A 1
H8A H 0.1191 0.8843 0.9318 0.060 Uiso 0.50 1 calc PR A 1
H8B H 0.1911 0.8619 1.0364 0.060 Uiso 0.50 1 calc PR A 1
C9 C 0.372(3) 0.8193(11) 0.9249(12) 0.048(2) Uani 0.50 1 d PDU A 1
H9A H 0.4689 0.8212 0.9614 0.058 Uiso 0.50 1 calc PR A 1
H9B H 0.3487 0.7444 0.9325 0.058 Uiso 0.50 1 calc PR A 1
C10 C 0.4134(16) 0.8641(10) 0.8143(10) 0.040(3) Uani 0.50 1 d PDU A 1
H10A H 0.3149 0.8622 0.7781 0.048 Uiso 0.50 1 calc PR A 1
C5A C 0.3986(18) 0.9783(12) 0.7834(8) 0.038(4) Uani 0.50 1 d PD A 2
H5AA H 0.2972 0.9593 0.7593 0.045 Uiso 0.50 1 calc PR A 2
C6A C 0.341(2) 1.0614(9) 0.8532(12) 0.042(4) Uani 0.50 1 d PD A 2
H6AA H 0.2870 1.1278 0.8163 0.050 Uiso 0.50 1 calc PR A 2
H6AB H 0.4378 1.0791 0.8813 0.050 Uiso 0.50 1 calc PR A 2
C7A C 0.214(2) 1.0129(13) 0.9373(12) 0.047(4) Uani 0.50 1 d PD A 2
H7AA H 0.1796 1.0642 0.9829 0.057 Uiso 0.50 1 calc PR A 2
H7AB H 0.1131 1.0003 0.9092 0.057 Uiso 0.50 1 calc PR A 2
C8A C 0.293(2) 0.9058(13) 0.9939(8) 0.050(4) Uani 0.50 1 d PD A 2
H8AA H 0.2097 0.8749 1.0440 0.060 Uiso 0.50 1 calc PR A 2
H8AB H 0.3870 0.9198 1.0275 0.060 Uiso 0.50 1 calc PR A 2
C9A C 0.358(3) 0.8236(10) 0.9239(13) 0.048(2) Uani 0.50 1 d PD A 2
H9AA H 0.2640 0.8047 0.8942 0.058 Uiso 0.50 1 calc PR A 2
H9AB H 0.4125 0.7578 0.9613 0.058 Uiso 0.50 1 calc PR A 2
C10A C 0.4869(18) 0.8739(10) 0.8416(9) 0.040(3) Uani 0.50 1 d PD A 2
H10B H 0.5789 0.8943 0.8738 0.048 Uiso 0.50 1 calc PR A 2
C11 C 0.5996(11) 0.7064(8) 0.7746(7) 0.044(2) Uani 1 1 d . A .
H11 H 0.5547 0.6581 0.8274 0.053 Uiso 1 1 calc R . .
C12 C 0.7182(11) 0.6707(7) 0.6942(7) 0.0418(19) Uani 1 1 d . A .
C13 C 0.7897(12) 0.5733(7) 0.6687(7) 0.047(2) Uani 1 1 d . A .
H13 H 0.7712 0.5050 0.7040 0.057 Uiso 1 1 calc R . .
C14 C 0.8780(12) 0.7020(7) 0.5595(6) 0.044(2) Uani 1 1 d . A .
H14 H 0.9345 0.7386 0.5031 0.052 Uiso 1 1 calc R . .
N7 N 0.8475(12) 0.3450(7) 0.2380(7) 0.052(2) Uani 0.50 1 d P . 1
N8 N 0.4626(12) 0.6705(7) 0.2075(8) 0.056(2) Uani 0.50 1 d P B 1
N9 N 0.1061(10) 0.9823(7) 0.2403(6) 0.0444(18) Uani 0.50 1 d P . 1
N10 N -0.0297(11) 0.7322(7) 0.2828(7) 0.050(2) Uani 0.50 1 d P . 1
C15 C 0.7757(11) 0.4290(7) 0.2183(7) 0.050(2) Uani 0.50 1 d P . 1
C16 C 0.3547(11) 0.7364(6) 0.2171(7) 0.049(2) Uani 0.50 1 d P B 1
C17 C 0.0665(9) 1.0718(6) 0.2481(5) 0.0364(16) Uani 0.50 1 d P . 1
C18 C -0.1282(13) 0.6750(8) 0.3177(7) 0.055(2) Uani 0.50 1 d P . 1
C7' C 0.8475(12) 0.3450(7) 0.2380(7) 0.052(2) Uani 0.50 1 d P . 2
C8' C 0.4626(12) 0.6705(7) 0.2075(8) 0.056(2) Uani 0.50 1 d P B 2
C9' C 0.1061(10) 0.9823(7) 0.2403(6) 0.0444(18) Uani 0.50 1 d P . 2
C10' C -0.0297(11) 0.7322(7) 0.2828(7) 0.050(2) Uani 0.50 1 d P . 2
N15' N 0.7757(11) 0.4290(7) 0.2183(7) 0.050(2) Uani 0.50 1 d P . 2
N16' N 0.3547(11) 0.7364(6) 0.2171(7) 0.049(2) Uani 0.50 1 d P B 2
N17' N 0.0665(9) 1.0718(6) 0.2481(5) 0.0364(16) Uani 0.50 1 d P . 2
N18' N -0.1282(13) 0.6750(8) 0.3177(7) 0.055(2) Uani 0.50 1 d P . 2
N11 N 0.5467(13) 0.5204(9) 0.4715(8) 0.067(3) Uani 0.50 1 d P . .
C11' C 0.5467(13) 0.5204(9) 0.4715(8) 0.067(3) Uani 0.50 1 d P . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 C7' 1.875(9) 1_565 ?
Cu1 N7 1.875(9) 1_565 ?
Cu1 N17' 1.934(7) 1_655 ?
Cu1 C17 1.934(7) 1_655 ?
Cu1 N1 2.033(7) . ?
Cu2 N6 1.854(7) 2_766 ?
Cu2 N6 1.854(7) . ?
Cu2 Cu3 2.8918(18) . ?
Cu2 Cu3 2.8918(18) 2_766 ?
Cu3 N18' 1.846(10) 1_655 ?
Cu3 C18 1.846(10) 1_655 ?
Cu3 N11 1.862(9) . ?
Cu3 Cu4 2.798(3) . ?
Cu4 C15 1.832(8) . ?
Cu4 N8 1.854(9) . ?
Cu5 N9 1.892(9) . ?
Cu5 C16 1.934(8) . ?
Cu5 N10 1.972(8) . ?
Cu6 N2 1.938(6) . ?
Cu6 N3 1.950(7) . ?
Cu6 N5 1.956(6) . ?
Cu6 N4 1.956(7) . ?
N1 C1 1.327(10) . ?
N1 C2 1.367(12) . ?
N2 C1 1.329(10) . ?
N2 C3 1.388(10) . ?
N3 C4 1.272(11) . ?
N3 C5A 1.452(11) . ?
N3 C5 1.463(11) . ?
N4 C11 1.247(11) . ?
N4 C10 1.471(11) . ?
N4 C10A 1.481(11) . ?
N5 C12 1.354(11) . ?
N5 C14 1.325(10) . ?
N6 C13 1.346(12) . ?
N6 C14 1.346(11) . ?
C1 H1 0.9300 . ?
C2 C3 1.371(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.440(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.537(9) . ?
C5 C10 1.541(9) . ?
C5 H5 0.9800 . ?
C6 C7 1.539(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.536(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.542(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.537(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9800 . ?
C5A C6A 1.535(9) . ?
C5A C10A 1.539(9) . ?
C5A H5AA 0.9800 . ?
C6A C7A 1.543(9) . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C7A C8A 1.529(9) . ?
C7A H7AA 0.9700 . ?
C7A H7AB 0.9700 . ?
C8A C9A 1.536(9) . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C9A C10A 1.544(9) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C10A H10B 0.9800 . ?
C11 C12 1.466(12) . ?
C11 H11 0.9300 . ?
C12 C13 1.369(12) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
N7 C15 1.138(11) . ?
N7 Cu1 1.875(9) 1_545 ?
N8 C16 1.129(12) . ?
N9 C17 1.150(11) . ?
N10 C18 1.142(12) . ?
C17 Cu1 1.934(7) 1_455 ?
C18 Cu3 1.846(10) 1_455 ?
N11 C11' 1.122(19) 2_666 ?
N11 N11 1.122(19) 2_666 ?

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
C7' Cu1 N7 0.0(8) 1_565 1_565 ?
C7' Cu1 N17' 145.0(4) 1_565 1_655 ?
N7 Cu1 N17' 145.0(4) 1_565 1_655 ?
C7' Cu1 C17 145.0(4) 1_565 1_655 ?
N7 Cu1 C17 145.0(4) 1_565 1_655 ?
N17' Cu1 C17 0.0(5) 1_655 1_655 ?
C7' Cu1 N1 112.2(4) 1_565 . ?
N7 Cu1 N1 112.2(4) 1_565 . ?
N17' Cu1 N1 101.5(3) 1_655 . ?
C17 Cu1 N1 101.5(3) 1_655 . ?
N6 Cu2 N6 180.000(2) 2_766 . ?
N6 Cu2 Cu3 98.0(3) 2_766 . ?
N6 Cu2 Cu3 82.0(3) . . ?
N6 Cu2 Cu3 82.0(3) 2_766 2_766 ?
N6 Cu2 Cu3 98.0(3) . 2_766 ?
Cu3 Cu2 Cu3 180.0 . 2_766 ?
N18' Cu3 C18 0.0(8) 1_655 1_655 ?
N18' Cu3 N11 168.2(5) 1_655 . ?
C18 Cu3 N11 168.2(5) 1_655 . ?
N18' Cu3 Cu4 87.3(3) 1_655 . ?
C18 Cu3 Cu4 87.3(3) 1_655 . ?
N11 Cu3 Cu4 101.4(4) . . ?
N18' Cu3 Cu2 81.4(3) 1_655 . ?
C18 Cu3 Cu2 81.4(3) 1_655 . ?
N11 Cu3 Cu2 98.1(4) . . ?
Cu4 Cu3 Cu2 132.19(7) . . ?
C15 Cu4 N8 168.2(4) . . ?
C15 Cu4 Cu3 86.8(3) . . ?
N8 Cu4 Cu3 87.4(3) . . ?
N9 Cu5 C16 132.0(4) . . ?
N9 Cu5 N10 122.6(4) . . ?
C16 Cu5 N10 105.3(4) . . ?
N2 Cu6 N3 83.0(3) . . ?
N2 Cu6 N5 112.4(3) . . ?
N3 Cu6 N5 163.8(3) . . ?
N2 Cu6 N4 164.7(3) . . ?
N3 Cu6 N4 82.3(3) . . ?
N5 Cu6 N4 81.8(3) . . ?
C1 N1 C2 103.8(7) . . ?
C1 N1 Cu1 124.9(6) . . ?
C2 N1 Cu1 131.2(6) . . ?
C1 N2 C3 104.4(6) . . ?
C1 N2 Cu6 144.3(6) . . ?
C3 N2 Cu6 111.1(5) . . ?
C4 N3 C5A 127.9(8) . . ?
C4 N3 C5 130.1(8) . . ?
C5A N3 C5 21.7(8) . . ?
C4 N3 Cu6 115.4(5) . . ?
C5A N3 Cu6 115.8(7) . . ?
C5 N3 Cu6 112.8(7) . . ?
C11 N4 C10 126.1(9) . . ?
C11 N4 C10A 129.7(9) . . ?
C10 N4 C10A 30.0(8) . . ?
C11 N4 Cu6 116.5(6) . . ?
C10 N4 Cu6 113.6(7) . . ?
C10A N4 Cu6 112.4(7) . . ?
C12 N5 C14 105.5(7) . . ?
C12 N5 Cu6 111.6(5) . . ?
C14 N5 Cu6 142.5(6) . . ?
C13 N6 C14 105.0(7) . . ?
C13 N6 Cu2 130.9(6) . . ?
C14 N6 Cu2 123.2(6) . . ?
N1 C1 N2 115.0(7) . . ?
N1 C1 H1 122.5 . . ?
N2 C1 H1 122.5 . . ?
C3 C2 N1 109.8(8) . . ?
C3 C2 H2 125.1 . . ?
N1 C2 H2 125.1 . . ?
C2 C3 N2 107.0(7) . . ?
C2 C3 C4 137.6(8) . . ?
N2 C3 C4 115.3(7) . . ?
N3 C4 C3 115.2(7) . . ?
N3 C4 H4 122.4 . . ?
C3 C4 H4 122.4 . . ?
N3 C5 C6 117.6(11) . . ?
N3 C5 C10 105.3(10) . . ?
C6 C5 C10 109.2(8) . . ?
N3 C5 H5 108.1 . . ?
C6 C5 H5 108.1 . . ?
C10 C5 H5 108.1 . . ?
C5 C6 C7 110.1(8) . . ?
C5 C6 H6A 109.6 . . ?
C7 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
C7 C6 H6B 109.6 . . ?
H6A C6 H6B 108.2 . . ?
C8 C7 C6 110.7(8) . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 C9 110.3(8) . . ?
C7 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C8 109.2(9) . . ?
C10 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
N4 C10 C9 114.8(11) . . ?
N4 C10 C5 104.5(10) . . ?
C9 C10 C5 109.9(8) . . ?
N4 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C5 C10 H10A 109.2 . . ?
N3 C5A C6A 117.1(12) . . ?
N3 C5A C10A 106.4(10) . . ?
C6A C5A C10A 109.8(8) . . ?
N3 C5A H5AA 107.7 . . ?
C6A C5A H5AA 107.7 . . ?
C10A C5A H5AA 107.7 . . ?
C5A C6A C7A 109.2(8) . . ?
C5A C6A H6AA 109.8 . . ?
C7A C6A H6AA 109.8 . . ?
C5A C6A H6AB 109.8 . . ?
C7A C6A H6AB 109.8 . . ?
H6AA C6A H6AB 108.3 . . ?
C8A C7A C6A 110.7(8) . . ?
C8A C7A H7AA 109.5 . . ?
C6A C7A H7AA 109.5 . . ?
C8A C7A H7AB 109.5 . . ?
C6A C7A H7AB 109.5 . . ?
H7AA C7A H7AB 108.1 . . ?
C7A C8A C9A 111.6(9) . . ?
C7A C8A H8AA 109.3 . . ?
C9A C8A H8AA 109.3 . . ?
C7A C8A H8AB 109.3 . . ?
C9A C8A H8AB 109.3 . . ?
H8AA C8A H8AB 108.0 . . ?
C8A C9A C10A 109.5(9) . . ?
C8A C9A H9AA 109.8 . . ?
C10A C9A H9AA 109.8 . . ?
C8A C9A H9AB 109.8 . . ?
C10A C9A H9AB 109.8 . . ?
H9AA C9A H9AB 108.2 . . ?
N4 C10A C5A 106.0(10) . . ?
N4 C10A C9A 117.7(11) . . ?
C5A C10A C9A 108.9(8) . . ?
N4 C10A H10B 108.0 . . ?
C5A C10A H10B 108.0 . . ?
C9A C10A H10B 108.0 . . ?
N4 C11 C12 114.4(8) . . ?
N4 C11 H11 122.8 . . ?
C12 C11 H11 122.8 . . ?
N5 C12 C13 108.2(7) . . ?
N5 C12 C11 115.4(7) . . ?
C13 C12 C11 136.5(8) . . ?
N6 C13 C12 108.7(8) . . ?
N6 C13 H13 125.7 . . ?
C12 C13 H13 125.7 . . ?
N5 C14 N6 112.6(7) . . ?
N5 C14 H14 123.7 . . ?
N6 C14 H14 123.7 . . ?
C15 N7 Cu1 169.5(9) . 1_545 ?
C16 N8 Cu4 175.2(10) . . ?
C17 N9 Cu5 172.1(7) . . ?
C18 N10 Cu5 171.7(9) . . ?
N7 C15 Cu4 170.5(9) . . ?
N8 C16 Cu5 170.8(8) . . ?
N9 C17 Cu1 159.5(7) . 1_455 ?
N10 C18 Cu3 174.3(9) . 1_455 ?
C11' N11 N11 0.0(11) 2_666 2_666 ?
C11' N11 Cu3 174.8(15) 2_666 . ?
N11 N11 Cu3 174.8(15) 2_666 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 Cu2 Cu3 N18' -82.2(4) 2_766 . . 1_655 ?
N6 Cu2 Cu3 N18' 97.8(4) . . . 1_655 ?
Cu3 Cu2 Cu3 N18' 159(100) 2_766 . . 1_655 ?
N6 Cu2 Cu3 C18 -82.2(4) 2_766 . . 1_655 ?
N6 Cu2 Cu3 C18 97.8(4) . . . 1_655 ?
Cu3 Cu2 Cu3 C18 159(100) 2_766 . . 1_655 ?
N6 Cu2 Cu3 N11 109.8(4) 2_766 . . . ?
N6 Cu2 Cu3 N11 -70.2(4) . . . . ?
Cu3 Cu2 Cu3 N11 -9(100) 2_766 . . . ?
N6 Cu2 Cu3 Cu4 -3.7(2) 2_766 . . . ?
N6 Cu2 Cu3 Cu4 176.3(2) . . . . ?
Cu3 Cu2 Cu3 Cu4 -122(100) 2_766 . . . ?
N18' Cu3 Cu4 C15 96.9(4) 1_655 . . . ?
C18 Cu3 Cu4 C15 96.9(4) 1_655 . . . ?
N11 Cu3 Cu4 C15 -91.2(5) . . . . ?
Cu2 Cu3 Cu4 C15 21.0(3) . . . . ?
N18' Cu3 Cu4 N8 -93.3(4) 1_655 . . . ?
C18 Cu3 Cu4 N8 -93.3(4) 1_655 . . . ?
N11 Cu3 Cu4 N8 78.6(5) . . . . ?
Cu2 Cu3 Cu4 N8 -169.2(3) . . . . ?
C7' Cu1 N1 C1 171.4(7) 1_565 . . . ?
N7 Cu1 N1 C1 171.4(7) 1_565 . . . ?
N17' Cu1 N1 C1 1.0(8) 1_655 . . . ?
C17 Cu1 N1 C1 1.0(8) 1_655 . . . ?
C7' Cu1 N1 C2 -12.3(10) 1_565 . . . ?
N7 Cu1 N1 C2 -12.3(10) 1_565 . . . ?
N17' Cu1 N1 C2 177.3(9) 1_655 . . . ?
C17 Cu1 N1 C2 177.3(9) 1_655 . . . ?
N3 Cu6 N2 C1 174.7(11) . . . . ?
N5 Cu6 N2 C1 -10.3(12) . . . . ?
N4 Cu6 N2 C1 -168.7(11) . . . . ?
N3 Cu6 N2 C3 1.4(6) . . . . ?
N5 Cu6 N2 C3 176.4(6) . . . . ?
N4 Cu6 N2 C3 18.0(15) . . . . ?
N2 Cu6 N3 C4 -0.4(6) . . . . ?
N5 Cu6 N3 C4 -163.4(10) . . . . ?
N4 Cu6 N3 C4 -176.1(7) . . . . ?
N2 Cu6 N3 C5A 169.2(9) . . . . ?
N5 Cu6 N3 C5A 6.1(15) . . . . ?
N4 Cu6 N3 C5A -6.5(8) . . . . ?
N2 Cu6 N3 C5 -167.2(8) . . . . ?
N5 Cu6 N3 C5 29.8(15) . . . . ?
N4 Cu6 N3 C5 17.2(8) . . . . ?
N2 Cu6 N4 C11 155.7(10) . . . . ?
N3 Cu6 N4 C11 172.3(8) . . . . ?
N5 Cu6 N4 C11 -4.2(7) . . . . ?
N2 Cu6 N4 C10 -3.8(17) . . . . ?
N3 Cu6 N4 C10 12.8(8) . . . . ?
N5 Cu6 N4 C10 -163.7(9) . . . . ?
N2 Cu6 N4 C10A -36.4(16) . . . . ?
N3 Cu6 N4 C10A -19.9(8) . . . . ?
N5 Cu6 N4 C10A 163.7(8) . . . . ?
N2 Cu6 N5 C12 -169.5(6) . . . . ?
N3 Cu6 N5 C12 -7.7(15) . . . . ?
N4 Cu6 N5 C12 4.9(6) . . . . ?
N2 Cu6 N5 C14 1.4(12) . . . . ?
N3 Cu6 N5 C14 163.2(10) . . . . ?
N4 Cu6 N5 C14 175.8(12) . . . . ?
N6 Cu2 N6 C13 3(100) 2_766 . . . ?
Cu3 Cu2 N6 C13 99.9(9) . . . . ?
Cu3 Cu2 N6 C13 -80.1(9) 2_766 . . . ?
N6 Cu2 N6 C14 -166(100) 2_766 . . . ?
Cu3 Cu2 N6 C14 -68.1(8) . . . . ?
Cu3 Cu2 N6 C14 111.9(8) 2_766 . . . ?
C2 N1 C1 N2 -0.1(11) . . . . ?
Cu1 N1 C1 N2 177.1(6) . . . . ?
C3 N2 C1 N1 0.6(10) . . . . ?
Cu6 N2 C1 N1 -173.0(8) . . . . ?
C1 N1 C2 C3 -0.4(11) . . . . ?
Cu1 N1 C2 C3 -177.3(7) . . . . ?
N1 C2 C3 N2 0.7(11) . . . . ?
N1 C2 C3 C4 177.3(10) . . . . ?
C1 N2 C3 C2 -0.8(10) . . . . ?
Cu6 N2 C3 C2 175.2(6) . . . . ?
C1 N2 C3 C4 -178.2(8) . . . . ?
Cu6 N2 C3 C4 -2.2(9) . . . . ?
C5A N3 C4 C3 -168.8(10) . . . . ?
C5 N3 C4 C3 163.3(10) . . . . ?
Cu6 N3 C4 C3 -0.7(10) . . . . ?
C2 C3 C4 N3 -174.3(11) . . . . ?
N2 C3 C4 N3 2.0(12) . . . . ?
C4 N3 C5 C6 32.7(17) . . . . ?
C5A N3 C5 C6 -60(3) . . . . ?
Cu6 N3 C5 C6 -163.0(10) . . . . ?
C4 N3 C5 C10 154.5(10) . . . . ?
C5A N3 C5 C10 62(3) . . . . ?
Cu6 N3 C5 C10 -41.1(12) . . . . ?
N3 C5 C6 C7 178.6(13) . . . . ?
C10 C5 C6 C7 58.8(15) . . . . ?
C5 C6 C7 C8 -57.5(16) . . . . ?
C6 C7 C8 C9 57.3(17) . . . . ?
C7 C8 C9 C10 -58.5(17) . . . . ?
C11 N4 C10 C9 45.2(17) . . . . ?
C10A N4 C10 C9 -63.4(18) . . . . ?
Cu6 N4 C10 C9 -157.6(11) . . . . ?
C11 N4 C10 C5 165.6(10) . . . . ?
C10A N4 C10 C5 57.0(16) . . . . ?
Cu6 N4 C10 C5 -37.2(12) . . . . ?
C8 C9 C10 N4 177.9(13) . . . . ?
C8 C9 C10 C5 60.5(16) . . . . ?
N3 C5 C10 N4 48.5(13) . . . . ?
C6 C5 C10 N4 175.6(11) . . . . ?
N3 C5 C10 C9 172.1(12) . . . . ?
C6 C5 C10 C9 -60.8(14) . . . . ?
C4 N3 C5A C6A -39.3(17) . . . . ?
C5 N3 C5A C6A 65(3) . . . . ?
Cu6 N3 C5A C6A 152.6(10) . . . . ?
C4 N3 C5A C10A -162.5(10) . . . . ?
C5 N3 C5A C10A -58(2) . . . . ?
Cu6 N3 C5A C10A 29.4(13) . . . . ?
N3 C5A C6A C7A 177.9(13) . . . . ?
C10A C5A C6A C7A -60.6(14) . . . . ?
C5A C6A C7A C8A 57.2(16) . . . . ?
C6A C7A C8A C9A -56.1(17) . . . . ?
C7A C8A C9A C10A 57.0(18) . . . . ?
C11 N4 C10A C5A -154.3(11) . . . . ?
C10 N4 C10A C5A -59.0(17) . . . . ?
Cu6 N4 C10A C5A 39.9(12) . . . . ?
C11 N4 C10A C9A -32.2(18) . . . . ?
C10 N4 C10A C9A 63.1(19) . . . . ?
Cu6 N4 C10A C9A 162.0(11) . . . . ?
N3 C5A C10A N4 -42.8(14) . . . . ?
C6A C5A C10A N4 -170.5(11) . . . . ?
N3 C5A C10A C9A -170.3(12) . . . . ?
C6A C5A C10A C9A 62.0(14) . . . . ?
C8A C9A C10A N4 -179.8(14) . . . . ?
C8A C9A C10A C5A -59.3(16) . . . . ?
C10 N4 C11 C12 159.0(10) . . . . ?
C10A N4 C11 C12 -162.9(11) . . . . ?
Cu6 N4 C11 C12 2.4(11) . . . . ?
C14 N5 C12 C13 0.2(11) . . . . ?
Cu6 N5 C12 C13 174.5(7) . . . . ?
C14 N5 C12 C11 -179.4(8) . . . . ?
Cu6 N5 C12 C11 -5.1(10) . . . . ?
N4 C11 C12 N5 1.9(13) . . . . ?
N4 C11 C12 C13 -177.6(11) . . . . ?
C14 N6 C13 C12 -0.4(11) . . . . ?
Cu2 N6 C13 C12 -170.1(7) . . . . ?
N5 C12 C13 N6 0.1(11) . . . . ?
C11 C12 C13 N6 179.6(11) . . . . ?
C12 N5 C14 N6 -0.5(11) . . . . ?
Cu6 N5 C14 N6 -171.7(8) . . . . ?
C13 N6 C14 N5 0.6(11) . . . . ?
Cu2 N6 C14 N5 171.3(6) . . . . ?
C15 Cu4 N8 C16 -1(13) . . . . ?
Cu3 Cu4 N8 C16 -61(11) . . . . ?
C16 Cu5 N9 C17 -144(6) . . . . ?
N10 Cu5 N9 C17 31(6) . . . . ?
N9 Cu5 N10 C18 -86(6) . . . . ?
C16 Cu5 N10 C18 91(6) . . . . ?
Cu1 N7 C15 Cu4 8(10) 1_545 . . . ?
N8 Cu4 C15 N7 15(7) . . . . ?
Cu3 Cu4 C15 N7 75(6) . . . . ?
Cu4 N8 C16 Cu5 -33(16) . . . . ?
N9 Cu5 C16 N8 169(6) . . . . ?
N10 Cu5 C16 N8 -8(6) . . . . ?
Cu5 N9 C17 Cu1 -22(7) . . . 1_455 ?
Cu5 N10 C18 Cu3 18(14) . . . 1_455 ?
N18' Cu3 N11 C11' -64(19) 1_655 . . 2_666 ?
C18 Cu3 N11 C11' -64(19) 1_655 . . 2_666 ?
Cu4 Cu3 N11 C11' 159(18) . . . 2_666 ?
Cu2 Cu3 N11 C11' 23(18) . . . 2_666 ?
N18' Cu3 N11 N11 -64(19) 1_655 . . 2_666 ?
C18 Cu3 N11 N11 -64(19) 1_655 . . 2_666 ?
Cu4 Cu3 N11 N11 159(18) . . . 2_666 ?
Cu2 Cu3 N11 N11 23(18) . . . 2_666 ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        27.59
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         1.751
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.162
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1048603'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H32 Cu9 N21 Ni2'
_chemical_formula_sum            'C37 H32 Cu9 N21 Ni2'
_chemical_formula_weight         1460.12

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'
Ni Ni 0.3393 1.1124 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0519(6)
_cell_length_b                   12.4494(9)
_cell_length_c                   13.6971(10)
_cell_angle_alpha                79.532(6)
_cell_angle_beta                 83.882(6)
_cell_angle_gamma                82.718(6)
_cell_volume                     1334.35(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2494
_cell_measurement_theta_min      3.2410
_cell_measurement_theta_max      22.8960

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.1513
_exptl_crystal_size_mid          0.0803
_exptl_crystal_size_min          0.0605
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             718
_exptl_absorpt_coefficient_mu    4.243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.40725
_exptl_absorpt_correction_T_max  1.00000
_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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4471
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14726
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0990
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         27.56
_reflns_number_total             5954
_reflns_number_gt                3309
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.1055P)²+8.3563P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5954
_refine_ls_number_parameters     331
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.1499
_refine_ls_R_factor_gt           0.0836
_refine_ls_wR_factor_ref         0.2707
_refine_ls_wR_factor_gt          0.2320
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.93974(19) 1.18888(11) 0.28463(11) 0.0552(4) Uani 1 1 d . . .
Cu2 Cu 1.0000 0.5000 0.5000 0.0632(6) Uani 1 2 d S . .
Cu3 Cu 0.7145(2) 0.58415(16) 0.38512(16) 0.0909(7) Uani 1 1 d . . .
Cu4 Cu 0.6409(2) 0.54771(15) 0.20103(18) 0.0934(7) Uani 1 1 d . . .
Cu5 Cu 0.15594(19) 0.81830(12) 0.23756(11) 0.0581(4) Uani 1 1 d . . .
Ni1 Ni 0.65095(17) 0.89151(10) 0.64675(9) 0.0431(4) Uani 1 1 d . A .
N1 N 0.8039(13) 1.1280(8) 0.4133(7) 0.060(3) Uani 1 1 d . . .
N2 N 0.7114(11) 1.0020(7) 0.5378(6) 0.044(2) Uani 1 1 d . A .
N3 N 0.5153(10) 1.0096(7) 0.6951(6) 0.0411(19) Uani 1 1 d D . .
N4 N 0.5577(11) 0.8054(7) 0.7632(7) 0.051(2) Uani 1 1 d D . .
N5 N 0.7620(11) 0.7526(7) 0.6210(6) 0.045(2) Uani 1 1 d . . .
N6 N 0.8873(13) 0.5946(8) 0.5822(7) 0.059(2) Uani 1 1 d . . .
C1 C 0.8085(14) 1.0223(8) 0.4540(8) 0.047(2) Uani 1 1 d . . .
H1 H 0.8747 0.9671 0.4258 0.056 Uiso 1 1 calc R . .
C2 C 0.6893(14) 1.1802(9) 0.4744(9) 0.055(3) Uani 1 1 d . A .
H2 H 0.6562 1.2554 0.4647 0.066 Uiso 1 1 calc R . .
C3 C 0.6299(13) 1.1051(9) 0.5524(8) 0.046(2) Uani 1 1 d . . .
C4 C 0.5208(14) 1.1048(8) 0.6410(8) 0.049(3) Uani 1 1 d . A .
H4 H 0.4590 1.1680 0.6582 0.059 Uiso 1 1 calc R . .
C5 C 0.454(2) 0.9811(14) 0.7996(9) 0.049(5) Uani 0.50 1 d PDU A 1
H5 H 0.5476 0.9821 0.8399 0.058 Uiso 0.50 1 calc PR A 1
C6 C 0.303(3) 1.0540(12) 0.8386(14) 0.049(5) Uani 0.50 1 d PDU A 1
H6A H 0.2096 1.0553 0.7992 0.059 Uiso 0.50 1 calc PR A 1
H6B H 0.3317 1.1285 0.8318 0.059 Uiso 0.50 1 calc PR A 1
C7 C 0.251(3) 1.0109(14) 0.9484(14) 0.059(5) Uani 0.50 1 d PDU A 1
H7A H 0.1516 1.0556 0.9704 0.070 Uiso 0.50 1 calc PR A 1
H7B H 0.3407 1.0168 0.9888 0.070 Uiso 0.50 1 calc PR A 1
C8 C 0.215(2) 0.8906(15) 0.9632(12) 0.058(5) Uani 0.50 1 d PDU A 1
H8A H 0.1194 0.8855 0.9277 0.070 Uiso 0.50 1 calc PR A 1
H8B H 0.1880 0.8641 1.0335 0.070 Uiso 0.50 1 calc PR A 1
C9 C 0.369(3) 0.8186(12) 0.9245(14) 0.054(3) Uani 0.50 1 d PDU A 1
H9A H 0.3446 0.7430 0.9332 0.065 Uiso 0.50 1 calc PR A 1
H9B H 0.4641 0.8207 0.9620 0.065 Uiso 0.50 1 calc PR A 1
C10 C 0.4132(19) 0.8620(13) 0.8131(11) 0.047(4) Uani 0.50 1 d PDU A 1
H10A H 0.3146 0.8611 0.7771 0.056 Uiso 0.50 1 calc PR A 1
C5A C 0.399(2) 0.9769(15) 0.7811(9) 0.049(5) Uani 0.50 1 d PD A 2
H5AA H 0.2984 0.9586 0.7562 0.058 Uiso 0.50 1 calc PR A 2
C6A C 0.342(3) 1.0590(11) 0.8525(14) 0.049(5) Uani 0.50 1 d PD A 2
H6AA H 0.2896 1.1269 0.8160 0.059 Uiso 0.50 1 calc PR A 2
H6AB H 0.4379 1.0756 0.8817 0.059 Uiso 0.50 1 calc PR A 2
C7A C 0.215(3) 1.0093(15) 0.9354(14) 0.059(5) Uani 0.50 1 d PD A 2
H7AA H 0.1801 1.0606 0.9812 0.070 Uiso 0.50 1 calc PR A 2
H7AB H 0.1157 0.9967 0.9063 0.070 Uiso 0.50 1 calc PR A 2
C8A C 0.294(2) 0.9003(15) 0.9924(9) 0.058(5) Uani 0.50 1 d PD A 2
H8AA H 0.2111 0.8686 1.0425 0.070 Uiso 0.50 1 calc PR A 2
H8AB H 0.3871 0.9140 1.0261 0.070 Uiso 0.50 1 calc PR A 2
C9A C 0.357(3) 0.8189(11) 0.9211(14) 0.054(3) Uani 0.50 1 d PD A 2
H9AA H 0.2624 0.8011 0.8907 0.065 Uiso 0.50 1 calc PR A 2
H9AB H 0.4093 0.7515 0.9580 0.065 Uiso 0.50 1 calc PR A 2
C10A C 0.485(2) 0.8701(13) 0.8394(11) 0.047(4) Uani 0.50 1 d PD A 2
H10B H 0.5766 0.8892 0.8720 0.056 Uiso 0.50 1 calc PR A 2
C11 C 0.5979(14) 0.7024(9) 0.7739(8) 0.052(3) Uani 1 1 d . A .
H11 H 0.5559 0.6532 0.8274 0.062 Uiso 1 1 calc R . .
C12 C 0.7172(15) 0.6684(8) 0.6936(8) 0.051(3) Uani 1 1 d . A .
C13 C 0.7913(15) 0.5725(9) 0.6668(8) 0.056(3) Uani 1 1 d . A .
H13 H 0.7769 0.5026 0.7021 0.067 Uiso 1 1 calc R . .
C14 C 0.8652(15) 0.7057(9) 0.5553(9) 0.054(3) Uani 1 1 d . A .
H14 H 0.9164 0.7440 0.4977 0.065 Uiso 1 1 calc R . .
N7 N 0.8538(15) 0.3367(10) 0.2411(9) 0.068(3) Uani 0.50 1 d P . 1
N8 N 0.4730(16) 0.6613(10) 0.2040(10) 0.070(3) Uani 0.50 1 d P B 1
N9 N 0.1103(13) 0.9730(9) 0.2363(8) 0.055(3) Uani 0.50 1 d P . 1
N10 N -0.0261(14) 0.7252(9) 0.2807(9) 0.061(3) Uani 0.50 1 d P . 1
C15 C 0.7829(14) 0.4213(9) 0.2207(8) 0.061(3) Uani 0.50 1 d P . 1
C16 C 0.3606(14) 0.7245(9) 0.2130(8) 0.057(3) Uani 0.50 1 d P B 1
C17 C 0.0707(13) 1.0604(9) 0.2458(8) 0.053(2) Uani 0.50 1 d P . 1
C18 C -0.1258(17) 0.6696(10) 0.3144(9) 0.070(3) Uani 0.50 1 d P . 1
C7' C 0.8538(15) 0.3367(10) 0.2411(9) 0.068(3) Uani 0.50 1 d P . 2
C8' C 0.4730(16) 0.6613(10) 0.2040(10) 0.070(3) Uani 0.50 1 d P B 2
C9' C 0.1103(13) 0.9730(9) 0.2363(8) 0.055(3) Uani 0.50 1 d P . 2
C10' C -0.0261(14) 0.7252(9) 0.2807(9) 0.061(3) Uani 0.50 1 d P . 2
N15' N 0.7829(14) 0.4213(9) 0.2207(8) 0.061(3) Uani 0.50 1 d P . 2
N16' N 0.3606(14) 0.7245(9) 0.2130(8) 0.057(3) Uani 0.50 1 d P B 2
N17' N 0.0707(13) 1.0604(9) 0.2458(8) 0.053(2) Uani 0.50 1 d P . 2
N18' N -0.1258(17) 0.6696(10) 0.3144(9) 0.070(3) Uani 0.50 1 d P . 2
N11 N 0.5454(16) 0.5217(12) 0.4725(10) 0.084(4) Uani 0.50 1 d P . .
C11' C 0.5454(16) 0.5217(12) 0.4725(10) 0.084(4) Uani 0.50 1 d P . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 C7' 1.894(12) 1_565 ?
Cu1 N7 1.894(12) 1_565 ?
Cu1 N17' 1.927(11) 1_655 ?
Cu1 C17 1.927(11) 1_655 ?
Cu1 N1 2.047(10) . ?
Cu2 N6 1.864(10) 2_766 ?
Cu2 N6 1.864(10) . ?
Cu2 Cu3 2.901(2) . ?
Cu2 Cu3 2.901(2) 2_766 ?
Cu3 N18' 1.852(13) 1_655 ?
Cu3 C18 1.852(13) 1_655 ?
Cu3 N11 1.864(11) . ?
Cu3 Cu4 2.778(3) . ?
Cu4 C15 1.819(11) . ?
Cu4 N8 1.831(13) . ?
Cu5 N9 1.912(11) . ?
Cu5 C16 1.931(12) . ?
Cu5 N10 1.959(11) . ?
Ni1 N4 1.893(8) . ?
Ni1 N3 1.893(8) . ?
Ni1 N2 1.904(8) . ?
Ni1 N5 1.917(8) . ?
N1 C1 1.330(13) . ?
N1 C2 1.362(15) . ?
N2 C1 1.321(13) . ?
N2 C3 1.404(13) . ?
N3 C4 1.282(13) . ?
N3 C5A 1.454(12) . ?
N3 C5 1.457(12) . ?
N4 C11 1.267(14) . ?
N4 C10 1.454(13) . ?
N4 C10A 1.462(13) . ?
N5 C14 1.323(13) . ?
N5 C12 1.363(13) . ?
N6 C13 1.328(15) . ?
N6 C14 1.358(14) . ?
C1 H1 0.9300 . ?
C2 C3 1.374(15) . ?
C2 H2 0.9300 . ?
C3 C4 1.419(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.532(9) . ?
C5 C10 1.535(9) . ?
C5 H5 0.9800 . ?
C6 C7 1.534(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.534(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.540(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.542(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9800 . ?
C5A C6A 1.538(9) . ?
C5A C10A 1.542(9) . ?
C5A H5AA 0.9800 . ?
C6A C7A 1.541(10) . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C7A C8A 1.535(10) . ?
C7A H7AA 0.9700 . ?
C7A H7AB 0.9700 . ?
C8A C9A 1.537(10) . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C9A C10A 1.543(10) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C10A H10B 0.9800 . ?
C11 C12 1.467(16) . ?
C11 H11 0.9300 . ?
C12 C13 1.359(16) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
N7 C15 1.136(14) . ?
N7 Cu1 1.894(12) 1_545 ?
N8 C16 1.134(15) . ?
N9 C17 1.121(14) . ?
N10 C18 1.133(15) . ?
C17 Cu1 1.927(11) 1_455 ?
C18 Cu3 1.852(13) 1_455 ?
N11 C11' 1.11(2) 2_666 ?
N11 N11 1.11(2) 2_666 ?

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
C7' Cu1 N7 0.0(10) 1_565 1_565 ?
C7' Cu1 N17' 145.3(5) 1_565 1_655 ?
N7 Cu1 N17' 145.3(5) 1_565 1_655 ?
C7' Cu1 C17 145.3(5) 1_565 1_655 ?
N7 Cu1 C17 145.3(5) 1_565 1_655 ?
N17' Cu1 C17 0.0(7) 1_655 1_655 ?
C7' Cu1 N1 109.1(5) 1_565 . ?
N7 Cu1 N1 109.1(5) 1_565 . ?
N17' Cu1 N1 103.7(4) 1_655 . ?
C17 Cu1 N1 103.7(4) 1_655 . ?
N6 Cu2 N6 180.000(2) 2_766 . ?
N6 Cu2 Cu3 98.9(3) 2_766 . ?
N6 Cu2 Cu3 81.1(3) . . ?
N6 Cu2 Cu3 81.1(3) 2_766 2_766 ?
N6 Cu2 Cu3 98.9(3) . 2_766 ?
Cu3 Cu2 Cu3 180.0 . 2_766 ?
N18' Cu3 C18 0.0(10) 1_655 1_655 ?
N18' Cu3 N11 167.9(6) 1_655 . ?
C18 Cu3 N11 167.9(6) 1_655 . ?
N18' Cu3 Cu4 86.1(4) 1_655 . ?
C18 Cu3 Cu4 86.1(4) 1_655 . ?
N11 Cu3 Cu4 103.1(5) . . ?
N18' Cu3 Cu2 80.1(4) 1_655 . ?
C18 Cu3 Cu2 80.1(4) 1_655 . ?
N11 Cu3 Cu2 99.2(5) . . ?
Cu4 Cu3 Cu2 130.88(9) . . ?
C15 Cu4 N8 168.2(5) . . ?
C15 Cu4 Cu3 87.5(4) . . ?
N8 Cu4 Cu3 87.1(4) . . ?
N9 Cu5 C16 132.6(5) . . ?
N9 Cu5 N10 119.0(5) . . ?
C16 Cu5 N10 108.2(5) . . ?
N4 Ni1 N3 84.1(4) . . ?
N4 Ni1 N2 168.0(4) . . ?
N3 Ni1 N2 84.0(4) . . ?
N4 Ni1 N5 83.5(4) . . ?
N3 Ni1 N5 167.5(4) . . ?
N2 Ni1 N5 108.3(4) . . ?
C1 N1 C2 104.4(9) . . ?
C1 N1 Cu1 125.0(8) . . ?
C2 N1 Cu1 130.5(8) . . ?
C1 N2 C3 104.8(8) . . ?
C1 N2 Ni1 144.7(8) . . ?
C3 N2 Ni1 110.3(6) . . ?
C4 N3 C5A 128.2(11) . . ?
C4 N3 C5 129.0(11) . . ?
C5A N3 C5 21.7(11) . . ?
C4 N3 Ni1 116.4(7) . . ?
C5A N3 Ni1 114.6(9) . . ?
C5 N3 Ni1 112.6(9) . . ?
C11 N4 C10 126.5(11) . . ?
C11 N4 C10A 127.8(11) . . ?
C10 N4 C10A 29.2(9) . . ?
C11 N4 Ni1 116.9(8) . . ?
C10 N4 Ni1 113.9(9) . . ?
C10A N4 Ni1 113.2(9) . . ?
C14 N5 C12 105.3(9) . . ?
C14 N5 Ni1 143.0(7) . . ?
C12 N5 Ni1 111.6(7) . . ?
C13 N6 C14 105.5(10) . . ?
C13 N6 Cu2 129.8(8) . . ?
C14 N6 Cu2 123.8(8) . . ?
N2 C1 N1 114.6(10) . . ?
N2 C1 H1 122.7 . . ?
N1 C1 H1 122.7 . . ?
N1 C2 C3 109.8(10) . . ?
N1 C2 H2 125.1 . . ?
C3 C2 H2 125.1 . . ?
C2 C3 N2 106.3(9) . . ?
C2 C3 C4 138.3(10) . . ?
N2 C3 C4 115.3(9) . . ?
N3 C4 C3 113.9(9) . . ?
N3 C4 H4 123.0 . . ?
C3 C4 H4 123.0 . . ?
N3 C5 C6 117.4(14) . . ?
N3 C5 C10 105.6(12) . . ?
C6 C5 C10 110.1(8) . . ?
N3 C5 H5 107.8 . . ?
C6 C5 H5 107.8 . . ?
C10 C5 H5 107.8 . . ?
C5 C6 C7 110.9(9) . . ?
C5 C6 H6A 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C6 C7 C8 111.0(9) . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 C9 110.5(9) . . ?
C7 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C8 C9 C10 109.3(9) . . ?
C8 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
C8 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
N4 C10 C5 104.3(12) . . ?
N4 C10 C9 117.5(13) . . ?
C5 C10 C9 109.7(9) . . ?
N4 C10 H10A 108.3 . . ?
C5 C10 H10A 108.3 . . ?
C9 C10 H10A 108.3 . . ?
N3 C5A C6A 118.4(14) . . ?
N3 C5A C10A 106.2(12) . . ?
C6A C5A C10A 109.4(8) . . ?
N3 C5A H5AA 107.5 . . ?
C6A C5A H5AA 107.5 . . ?
C10A C5A H5AA 107.5 . . ?
C5A C6A C7A 109.6(9) . . ?
C5A C6A H6AA 109.8 . . ?
C7A C6A H6AA 109.8 . . ?
C5A C6A H6AB 109.8 . . ?
C7A C6A H6AB 109.8 . . ?
H6AA C6A H6AB 108.2 . . ?
C8A C7A C6A 110.4(9) . . ?
C8A C7A H7AA 109.6 . . ?
C6A C7A H7AA 109.6 . . ?
C8A C7A H7AB 109.6 . . ?
C6A C7A H7AB 109.6 . . ?
H7AA C7A H7AB 108.1 . . ?
C7A C8A C9A 110.8(9) . . ?
C7A C8A H8AA 109.5 . . ?
C9A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
C9A C8A H8AB 109.5 . . ?
H8AA C8A H8AB 108.1 . . ?
C8A C9A C10A 109.8(9) . . ?
C8A C9A H9AA 109.7 . . ?
C10A C9A H9AA 109.7 . . ?
C8A C9A H9AB 109.7 . . ?
C10A C9A H9AB 109.7 . . ?
H9AA C9A H9AB 108.2 . . ?
N4 C10A C9A 118.1(13) . . ?
N4 C10A C5A 105.0(12) . . ?
C9A C10A C5A 109.2(9) . . ?
N4 C10A H10B 108.1 . . ?
C9A C10A H10B 108.1 . . ?
C5A C10A H10B 108.1 . . ?
N4 C11 C12 113.5(9) . . ?
N4 C11 H11 123.3 . . ?
C12 C11 H11 123.3 . . ?
C13 C12 N5 108.2(10) . . ?
C13 C12 C11 137.2(10) . . ?
N5 C12 C11 114.4(9) . . ?
N6 C13 C12 109.1(10) . . ?
N6 C13 H13 125.5 . . ?
C12 C13 H13 125.5 . . ?
N5 C14 N6 111.8(10) . . ?
N5 C14 H14 124.1 . . ?
N6 C14 H14 124.1 . . ?
C15 N7 Cu1 171.2(11) . 1_545 ?
C16 N8 Cu4 173.0(12) . . ?
C17 N9 Cu5 171.5(10) . . ?
C18 N10 Cu5 173.4(12) . . ?
N7 C15 Cu4 170.6(12) . . ?
N8 C16 Cu5 173.3(11) . . ?
N9 C17 Cu1 161.2(10) . 1_455 ?
N10 C18 Cu3 172.6(12) . 1_455 ?
C11' N11 N11 0.0(14) 2_666 2_666 ?
C11' N11 Cu3 174(2) 2_666 . ?
N11 N11 Cu3 174(2) 2_666 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 Cu2 Cu3 N18' -80.0(5) 2_766 . . 1_655 ?
N6 Cu2 Cu3 N18' 100.0(5) . . . 1_655 ?
Cu3 Cu2 Cu3 N18' 31(100) 2_766 . . 1_655 ?
N6 Cu2 Cu3 C18 -80.0(5) 2_766 . . 1_655 ?
N6 Cu2 Cu3 C18 100.0(5) . . . 1_655 ?
Cu3 Cu2 Cu3 C18 31(100) 2_766 . . 1_655 ?
N6 Cu2 Cu3 N11 112.3(6) 2_766 . . . ?
N6 Cu2 Cu3 N11 -67.7(6) . . . . ?
Cu3 Cu2 Cu3 N11 -137(100) 2_766 . . . ?
N6 Cu2 Cu3 Cu4 -4.0(3) 2_766 . . . ?
N6 Cu2 Cu3 Cu4 176.0(3) . . . . ?
Cu3 Cu2 Cu3 Cu4 107(100) 2_766 . . . ?
N18' Cu3 Cu4 C15 95.3(5) 1_655 . . . ?
C18 Cu3 Cu4 C15 95.3(5) 1_655 . . . ?
N11 Cu3 Cu4 C15 -92.8(6) . . . . ?
Cu2 Cu3 Cu4 C15 22.0(4) . . . . ?
N18' Cu3 Cu4 N8 -95.2(5) 1_655 . . . ?
C18 Cu3 Cu4 N8 -95.2(5) 1_655 . . . ?
N11 Cu3 Cu4 N8 76.7(6) . . . . ?
Cu2 Cu3 Cu4 N8 -168.6(4) . . . . ?
C7' Cu1 N1 C1 166.7(10) 1_565 . . . ?
N7 Cu1 N1 C1 166.7(10) 1_565 . . . ?
N17' Cu1 N1 C1 -1.8(11) 1_655 . . . ?
C17 Cu1 N1 C1 -1.8(11) 1_655 . . . ?
C7' Cu1 N1 C2 -11.3(12) 1_565 . . . ?
N7 Cu1 N1 C2 -11.3(12) 1_565 . . . ?
N17' Cu1 N1 C2 -179.9(11) 1_655 . . . ?
C17 Cu1 N1 C2 -179.9(11) 1_655 . . . ?
N4 Ni1 N2 C1 -176.5(17) . . . . ?
N3 Ni1 N2 C1 175.7(14) . . . . ?
N5 Ni1 N2 C1 -6.6(14) . . . . ?
N4 Ni1 N2 C3 9(2) . . . . ?
N3 Ni1 N2 C3 1.0(7) . . . . ?
N5 Ni1 N2 C3 178.7(7) . . . . ?
N4 Ni1 N3 C4 -179.0(8) . . . . ?
N2 Ni1 N3 C4 -0.6(8) . . . . ?
N5 Ni1 N3 C4 -170.6(15) . . . . ?
N4 Ni1 N3 C5A -8.1(10) . . . . ?
N2 Ni1 N3 C5A 170.3(10) . . . . ?
N5 Ni1 N3 C5A 0(2) . . . . ?
N4 Ni1 N3 C5 15.5(10) . . . . ?
N2 Ni1 N3 C5 -166.1(10) . . . . ?
N5 Ni1 N3 C5 24(2) . . . . ?
N3 Ni1 N4 C11 176.2(9) . . . . ?
N2 Ni1 N4 C11 168.4(16) . . . . ?
N5 Ni1 N4 C11 -1.9(9) . . . . ?
N3 Ni1 N4 C10 13.3(10) . . . . ?
N2 Ni1 N4 C10 5(2) . . . . ?
N5 Ni1 N4 C10 -164.9(10) . . . . ?
N3 Ni1 N4 C10A -18.6(10) . . . . ?
N2 Ni1 N4 C10A -26(2) . . . . ?
N5 Ni1 N4 C10A 163.2(10) . . . . ?
N4 Ni1 N5 C14 178.0(14) . . . . ?
N3 Ni1 N5 C14 169.5(14) . . . . ?
N2 Ni1 N5 C14 0.1(14) . . . . ?
N4 Ni1 N5 C12 1.3(8) . . . . ?
N3 Ni1 N5 C12 -7(2) . . . . ?
N2 Ni1 N5 C12 -176.6(7) . . . . ?
N6 Cu2 N6 C13 109(100) 2_766 . . . ?
Cu3 Cu2 N6 C13 101.7(12) . . . . ?
Cu3 Cu2 N6 C13 -78.3(12) 2_766 . . . ?
N6 Cu2 N6 C14 -59(100) 2_766 . . . ?
Cu3 Cu2 N6 C14 -65.8(10) . . . . ?
Cu3 Cu2 N6 C14 114.2(10) 2_766 . . . ?
C3 N2 C1 N1 2.0(13) . . . . ?
Ni1 N2 C1 N1 -172.9(9) . . . . ?
C2 N1 C1 N2 -2.2(14) . . . . ?
Cu1 N1 C1 N2 179.3(7) . . . . ?
C1 N1 C2 C3 1.5(13) . . . . ?
Cu1 N1 C2 C3 179.8(8) . . . . ?
N1 C2 C3 N2 -0.4(13) . . . . ?
N1 C2 C3 C4 175.8(13) . . . . ?
C1 N2 C3 C2 -0.9(12) . . . . ?
Ni1 N2 C3 C2 175.9(7) . . . . ?
C1 N2 C3 C4 -178.1(10) . . . . ?
Ni1 N2 C3 C4 -1.3(11) . . . . ?
C5A N3 C4 C3 -169.4(13) . . . . ?
C5 N3 C4 C3 162.7(13) . . . . ?
Ni1 N3 C4 C3 0.0(13) . . . . ?
C2 C3 C4 N3 -175.1(13) . . . . ?
N2 C3 C4 N3 0.8(14) . . . . ?
C4 N3 C5 C6 35(2) . . . . ?
C5A N3 C5 C6 -61(3) . . . . ?
Ni1 N3 C5 C6 -161.5(12) . . . . ?
C4 N3 C5 C10 158.3(12) . . . . ?
C5A N3 C5 C10 62(3) . . . . ?
Ni1 N3 C5 C10 -38.4(14) . . . . ?
N3 C5 C6 C7 178.0(16) . . . . ?
C10 C5 C6 C7 57.3(17) . . . . ?
C5 C6 C7 C8 -55.8(18) . . . . ?
C6 C7 C8 C9 56.5(18) . . . . ?
C7 C8 C9 C10 -58.6(18) . . . . ?
C11 N4 C10 C5 162.7(13) . . . . ?
C10A N4 C10 C5 59(2) . . . . ?
Ni1 N4 C10 C5 -36.3(14) . . . . ?
C11 N4 C10 C9 41(2) . . . . ?
C10A N4 C10 C9 -63(2) . . . . ?
Ni1 N4 C10 C9 -158.0(12) . . . . ?
N3 C5 C10 N4 46.0(16) . . . . ?
C6 C5 C10 N4 173.6(14) . . . . ?
N3 C5 C10 C9 172.7(14) . . . . ?
C6 C5 C10 C9 -59.7(16) . . . . ?
C8 C9 C10 N4 179.1(16) . . . . ?
C8 C9 C10 C5 60.2(17) . . . . ?
C4 N3 C5A C6A -37(2) . . . . ?
C5 N3 C5A C6A 64(3) . . . . ?
Ni1 N3 C5A C6A 153.9(12) . . . . ?
C4 N3 C5A C10A -159.8(12) . . . . ?
C5 N3 C5A C10A -59(3) . . . . ?
Ni1 N3 C5A C10A 30.6(15) . . . . ?
N3 C5A C6A C7A 177.9(15) . . . . ?
C10A C5A C6A C7A -60.5(16) . . . . ?
C5A C6A C7A C8A 58.1(17) . . . . ?
C6A C7A C8A C9A -56.9(18) . . . . ?
C7A C8A C9A C10A 57.6(18) . . . . ?
C11 N4 C10A C9A -36(2) . . . . ?
C10 N4 C10A C9A 63(2) . . . . ?
Ni1 N4 C10A C9A 160.5(12) . . . . ?
C11 N4 C10A C5A -158.3(13) . . . . ?
C10 N4 C10A C5A -59(2) . . . . ?
Ni1 N4 C10A C5A 38.6(14) . . . . ?
C8A C9A C10A N4 -179.3(16) . . . . ?
C8A C9A C10A C5A -59.5(17) . . . . ?
N3 C5A C10A N4 -42.4(16) . . . . ?
C6A C5A C10A N4 -171.2(14) . . . . ?
N3 C5A C10A C9A -169.9(14) . . . . ?
C6A C5A C10A C9A 61.3(16) . . . . ?
C10 N4 C11 C12 162.6(12) . . . . ?
C10A N4 C11 C12 -160.6(12) . . . . ?
Ni1 N4 C11 C12 2.1(14) . . . . ?
C14 N5 C12 C13 -2.2(13) . . . . ?
Ni1 N5 C12 C13 175.8(8) . . . . ?
C14 N5 C12 C11 -178.5(10) . . . . ?
Ni1 N5 C12 C11 -0.6(12) . . . . ?
N4 C11 C12 C13 -175.9(14) . . . . ?
N4 C11 C12 N5 -1.0(15) . . . . ?
C14 N6 C13 C12 -2.6(14) . . . . ?
Cu2 N6 C13 C12 -171.8(9) . . . . ?
N5 C12 C13 N6 3.0(14) . . . . ?
C11 C12 C13 N6 178.1(13) . . . . ?
C12 N5 C14 N6 0.6(13) . . . . ?
Ni1 N5 C14 N6 -176.2(10) . . . . ?
C13 N6 C14 N5 1.2(14) . . . . ?
Cu2 N6 C14 N5 171.3(8) . . . . ?
C15 Cu4 N8 C16 -10(12) . . . . ?
Cu3 Cu4 N8 C16 -73(10) . . . . ?
C16 Cu5 N9 C17 -139(7) . . . . ?
N10 Cu5 N9 C17 36(7) . . . . ?
N9 Cu5 N10 C18 -95(10) . . . . ?
C16 Cu5 N10 C18 81(10) . . . . ?
Cu1 N7 C15 Cu4 8(15) 1_545 . . . ?
N8 Cu4 C15 N7 16(9) . . . . ?
Cu3 Cu4 C15 N7 79(7) . . . . ?
Cu4 N8 C16 Cu5 -10(19) . . . . ?
N9 Cu5 C16 N8 157(10) . . . . ?
N10 Cu5 C16 N8 -18(10) . . . . ?
Cu5 N9 C17 Cu1 -24(9) . . . 1_455 ?
Cu5 N10 C18 Cu3 27(18) . . . 1_455 ?
N18' Cu3 N11 C11' -110(21) 1_655 . . 2_666 ?
C18 Cu3 N11 C11' -110(21) 1_655 . . 2_666 ?
Cu4 Cu3 N11 C11' 112(21) . . . 2_666 ?
Cu2 Cu3 N11 C11' -24(21) . . . 2_666 ?
N18' Cu3 N11 N11 -110(21) 1_655 . . 2_666 ?
C18 Cu3 N11 N11 -110(21) 1_655 . . 2_666 ?
Cu4 Cu3 N11 N11 112(21) . . . 2_666 ?
Cu2 Cu3 N11 N11 -24(21) . . . 2_666 ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.557
_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_4
_database_code_depnum_ccdc_archive 'CCDC 1048604'
_audit_update_record             
;
2015-02-09 deposited with the CCDC.
2015-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H18 Cu2 I2 N4'
_chemical_formula_sum            'C21 H18 Cu2 I2 N4'
_chemical_formula_weight         707.27

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           Orthorhombic
_symmetry_space_group_name_H-M   Cmca

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

_cell_length_a                   14.191
_cell_length_b                   21.044
_cell_length_c                   15.410
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4601.8
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5405
_cell_measurement_theta_min      2.8650
_cell_measurement_theta_max      28.0547

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2688
_exptl_absorpt_coefficient_mu    4.546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10458
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2113
_reflns_number_gt                1884
_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)+(0.0308P)²+12.9116P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2113
_refine_ls_number_parameters     139
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0617
_refine_ls_wR_factor_gt          0.0587
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_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 0.0000 0.182359(16) 0.05405(2) 0.04144(12) Uani 1 2 d S . .
I2 I 0.0000 0.024663(16) 0.25279(2) 0.03531(12) Uani 1 2 d S . .
Cu3 Cu 0.0000 0.05770(3) 0.08055(4) 0.03193(16) Uani 1 2 d S . .
Cu4 Cu 0.0000 0.14597(3) 0.21759(5) 0.0479(2) Uani 1 2 d S . .
N3 N 0.12193(18) 0.02346(11) 0.03448(16) 0.0219(6) Uani 1 1 d . . .
C11 C 0.2764(3) 0.0000 0.0000 0.0231(9) Uani 1 2 d S . .
C12 C 0.3396(2) 0.04627(16) -0.0529(2) 0.0298(8) Uani 1 1 d . . .
H12A H 0.3898 0.0615 -0.0156 0.036 Uiso 1 1 calc R . .
H12B H 0.3685 0.0229 -0.1002 0.036 Uiso 1 1 calc R . .
C14 C 0.2072(2) 0.03620(14) 0.05501(19) 0.0227(7) Uani 1 1 d . . .
C15 C 0.1935(3) 0.20898(17) -0.1544(2) 0.0354(8) Uani 1 1 d . . .
C16 C 0.2731(3) 0.21655(17) -0.1041(3) 0.0426(9) Uani 1 1 d . . .
H16 H 0.2954 0.2571 -0.0917 0.051 Uiso 1 1 calc R . .
C21 C 0.1615(3) 0.14850(18) -0.1743(2) 0.0391(9) Uani 1 1 d . . .
H21 H 0.1077 0.1432 -0.2079 0.047 Uiso 1 1 calc R . .
C22 C 0.2096(3) 0.09640(17) -0.1439(2) 0.0355(8) Uani 1 1 d . . .
H22 H 0.1895 0.0559 -0.1594 0.043 Uiso 1 1 calc R . .
C24 C 0.2881(2) 0.10313(16) -0.0903(2) 0.0288(7) Uani 1 1 d . . .
C25 C 0.3195(3) 0.16404(17) -0.0720(2) 0.0381(9) Uani 1 1 d . . .
H25 H 0.3727 0.1696 -0.0375 0.046 Uiso 1 1 calc R . .
C1 C 0.2344(2) 0.08213(16) 0.1237(2) 0.0326(8) Uani 1 1 d . . .
H1A H 0.2538 0.1213 0.0975 0.049 Uiso 1 1 calc R . .
H1B H 0.2855 0.0649 0.1572 0.049 Uiso 1 1 calc R . .
H1C H 0.1814 0.0898 0.1611 0.049 Uiso 1 1 calc R . .
C2 C 0.1450(3) 0.26314(19) -0.1897(3) 0.0432(9) Uani 1 1 d . . .
N1 N 0.1064(3) 0.30487(17) -0.2199(3) 0.0547(9) Uani 1 1 d . . .


_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 Cu4 2.6339(9) . ?
I1 Cu3 2.6548(7) . ?
I2 Cu4 2.6097(8) . ?
I2 Cu3 2.7437(7) . ?
Cu3 N3 2.004(3) . ?
Cu3 N3 2.004(3) 11 ?
Cu3 Cu4 2.8124(9) . ?
Cu4 N1 2.069(4) 12_566 ?
Cu4 N1 2.069(4) 2 ?
N3 C14 1.279(4) . ?
N3 N3 1.450(5) 3 ?
C11 C14 1.504(4) . ?
C11 C14 1.504(4) 3 ?
C11 C12 1.555(4) . ?
C11 C12 1.555(4) 3 ?
C12 C24 1.516(5) . ?
C14 C1 1.485(4) . ?
C15 C16 1.379(5) . ?
C15 C21 1.385(5) . ?
C15 C2 1.438(5) . ?
C16 C25 1.379(5) . ?
C21 C22 1.374(5) . ?
C22 C24 1.394(5) . ?
C24 C25 1.386(5) . ?
C2 N1 1.135(5) . ?
N1 Cu4 2.069(4) 2_554 ?

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
Cu4 I1 Cu3 64.25(2) . . ?
Cu4 I2 Cu3 63.32(2) . . ?
N3 Cu3 N3 119.37(14) . 11 ?
N3 Cu3 I1 107.51(7) . . ?
N3 Cu3 I1 107.51(7) 11 . ?
N3 Cu3 I2 104.57(7) . . ?
N3 Cu3 I2 104.57(7) 11 . ?
I1 Cu3 I2 113.53(2) . . ?
N3 Cu3 Cu4 120.23(7) . . ?
N3 Cu3 Cu4 120.23(7) 11 . ?
I1 Cu3 Cu4 57.51(2) . . ?
I2 Cu3 Cu4 56.01(2) . . ?
N1 Cu4 N1 93.8(2) 12_566 2 ?
N1 Cu4 I2 113.10(10) 12_566 . ?
N1 Cu4 I2 113.10(10) 2 . ?
N1 Cu4 I1 107.48(11) 12_566 . ?
N1 Cu4 I1 107.48(11) 2 . ?
I2 Cu4 I1 118.90(3) . . ?
N1 Cu4 Cu3 132.85(11) 12_566 . ?
N1 Cu4 Cu3 132.85(11) 2 . ?
I2 Cu4 Cu3 60.66(2) . . ?
I1 Cu4 Cu3 58.24(2) . . ?
C14 N3 N3 108.90(18) . 3 ?
C14 N3 Cu3 130.8(2) . . ?
N3 N3 Cu3 120.28(7) 3 . ?
C14 C11 C14 98.5(3) . 3 ?
C14 C11 C12 110.79(17) . . ?
C14 C11 C12 113.47(17) 3 . ?
C14 C11 C12 113.47(17) . 3 ?
C14 C11 C12 110.79(17) 3 3 ?
C12 C11 C12 109.5(4) . 3 ?
C24 C12 C11 114.5(3) . . ?
N3 C14 C1 124.0(3) . . ?
N3 C14 C11 111.8(3) . . ?
C1 C14 C11 124.2(3) . . ?
C16 C15 C21 119.9(3) . . ?
C16 C15 C2 120.9(3) . . ?
C21 C15 C2 119.2(3) . . ?
C15 C16 C25 120.1(3) . . ?
C22 C21 C15 119.7(3) . . ?
C21 C22 C24 121.2(3) . . ?
C25 C24 C22 118.1(3) . . ?
C25 C24 C12 119.8(3) . . ?
C22 C24 C12 122.0(3) . . ?
C16 C25 C24 121.0(4) . . ?
N1 C2 C15 177.8(4) . . ?
C2 N1 Cu4 158.5(4) . 2_554 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.084
