# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_11
_audit_block_doi                 10.5517/ccdc.csd.cc1ly0tc
_database_code_depnum_ccdc_archive 'CCDC 1487653'
_audit_update_record             
;
2016-07-14 deposited with the CCDC.
2016-07-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C114 H84 Cl4 Cu4 N24 O0'
_chemical_formula_sum            'C114 H84 Cl4 Cu4 N24 O0'
_chemical_formula_weight         2186.01

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   'Pn-3  '

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

_cell_length_a                   16.930(5)
_cell_length_b                   16.930(5)
_cell_length_c                   16.930(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4853(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1440
_cell_measurement_theta_min      0.7957
_cell_measurement_theta_max      0.8347

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2240
_exptl_absorpt_coefficient_mu    1.041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7957
_exptl_absorpt_correction_T_max  0.8347
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26520
_diffrn_reflns_av_R_equivalents  0.1007
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1440
_reflns_number_gt                1033
_reflns_threshold_expression     >2σ(I)

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

_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 > 2σ(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)+(0.1168P)²+10.4559P] 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         1440
_refine_ls_number_parameters     113
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0645
_refine_ls_wR_factor_ref         0.2095
_refine_ls_wR_factor_gt          0.1862
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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 0.33723(4) 0.16277(4) 0.16277(4) 0.0460(5) Uani 1 3 d S . .
Cl2 Cl 0.5000 0.0000 0.0000 0.0458(9) Uani 1 6 d S . .
N1 N 0.5195(2) 0.2579(2) 0.0290(2) 0.0314(10) Uani 1 1 d . . .
C7 C 0.5680(3) 0.2560(3) -0.0401(3) 0.0293(11) Uani 1 1 d . . .
N2 N 0.4336(3) 0.2220(3) 0.1202(3) 0.0472(12) Uani 1 1 d . . .
C2 C 0.6623(3) 0.2528(3) -0.1758(3) 0.0281(11) Uani 1 1 d . . .
C6 C 0.6275(3) 0.3107(3) -0.0503(3) 0.0345(12) Uani 1 1 d . . .
H6 H 0.6364 0.3488 -0.0118 0.041 Uiso 1 1 calc R . .
C4 C 0.6021(3) 0.1979(3) -0.1642(3) 0.0364(12) Uani 1 1 d . . .
H4 H 0.5929 0.1596 -0.2025 0.044 Uiso 1 1 calc R . .
C9 C 0.4693(4) 0.2020(3) 0.0541(4) 0.0483(15) Uani 1 1 d . . .
H9 H 0.4608 0.1545 0.0279 0.058 Uiso 1 1 calc R . .
C5 C 0.5558(3) 0.1992(3) -0.0970(3) 0.0396(13) Uani 1 1 d . . .
H5 H 0.5164 0.1616 -0.0902 0.047 Uiso 1 1 calc R . .
C1 C 0.7102(4) 0.2500 -0.2500 0.0274(14) Uani 1 2 d S . .
C3 C 0.6737(3) 0.3094(3) -0.1170(3) 0.0326(12) Uani 1 1 d . . .
H3 H 0.7134 0.3469 -0.1230 0.039 Uiso 1 1 calc R . .
C8 C 0.5155(4) 0.3173(4) 0.0848(4) 0.0541(17) Uani 1 1 d . . .
H8 H 0.5427 0.3650 0.0841 0.065 Uiso 1 1 calc R . .
C10 C 0.4645(4) 0.2926(4) 0.1405(4) 0.0530(16) Uani 1 1 d . . .
H10 H 0.4524 0.3202 0.1864 0.064 Uiso 1 1 calc R . .
Cl3 Cl 0.5000 0.5000 0.0000 0.125(5) Uani 0.50 6 d SP . .
Cl1 Cl 0.2500 0.2500 0.2500 0.0422(11) Uani 1 12 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0460(5) 0.0460(5) 0.0460(5) -0.0017(3) 0.0017(3) 0.0017(3)
Cl2 0.0458(9) 0.0458(9) 0.0458(9) -0.0066(8) 0.0066(8) 0.0066(8)
N1 0.027(2) 0.039(2) 0.029(2) -0.0013(18) 0.0064(17) 0.0001(18)
C7 0.032(3) 0.034(3) 0.021(2) 0.002(2) 0.0000(19) 0.007(2)
N2 0.049(3) 0.050(3) 0.042(3) -0.007(2) 0.017(2) -0.004(2)
C2 0.025(2) 0.037(3) 0.022(2) 0.001(2) 0.0007(19) 0.003(2)
C6 0.038(3) 0.036(3) 0.029(3) -0.009(2) -0.001(2) -0.003(2)
C4 0.038(3) 0.042(3) 0.028(3) -0.011(2) 0.003(2) -0.011(2)
C9 0.056(4) 0.042(3) 0.046(3) -0.011(3) 0.017(3) -0.010(3)
C5 0.036(3) 0.046(3) 0.037(3) -0.005(3) 0.004(2) -0.015(2)
C1 0.033(3) 0.027(3) 0.022(3) -0.001(3) 0.000 0.000
C3 0.030(3) 0.038(3) 0.029(3) -0.002(2) 0.004(2) -0.006(2)
C8 0.061(4) 0.049(3) 0.052(4) -0.021(3) 0.015(3) -0.016(3)
C10 0.059(4) 0.053(4) 0.047(3) -0.020(3) 0.019(3) -0.010(3)
Cl3 0.125(5) 0.125(5) 0.125(5) 0.019(5) 0.019(5) -0.019(5)
Cl1 0.0422(11) 0.0422(11) 0.0422(11) 0.000 0.000 0.000

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N2 2.047(5) 8 ?
Cu1 N2 2.047(5) 7 ?
Cu1 N2 2.047(5) . ?
Cu1 Cl1 2.5579(15) . ?
N1 C9 1.342(7) . ?
N1 C8 1.382(7) . ?
N1 C7 1.429(6) . ?
C7 C5 1.375(7) . ?
C7 C6 1.380(7) . ?
N2 C9 1.316(7) . ?
N2 C10 1.349(8) . ?
C2 C4 1.393(7) . ?
C2 C3 1.395(7) . ?
C2 C1 1.495(6) . ?
C6 C3 1.373(7) . ?
C4 C5 1.382(7) . ?
C1 C1 1.348(13) 2_655 ?
C1 C2 1.495(6) 3_554 ?
C8 C10 1.344(9) . ?
Cl1 Cu1 2.5579(15) 3 ?
Cl1 Cu1 2.5579(15) 4 ?
Cl1 Cu1 2.5579(15) 2 ?

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
N2 Cu1 N2 106.42(15) 8 7 ?
N2 Cu1 N2 106.42(15) 8 . ?
N2 Cu1 N2 106.42(15) 7 . ?
N2 Cu1 Cl1 112.37(13) 8 . ?
N2 Cu1 Cl1 112.37(13) 7 . ?
N2 Cu1 Cl1 112.37(13) . . ?
C9 N1 C8 105.4(4) . . ?
C9 N1 C7 127.3(4) . . ?
C8 N1 C7 127.3(5) . . ?
C5 C7 C6 119.4(4) . . ?
C5 C7 N1 120.2(5) . . ?
C6 C7 N1 120.4(4) . . ?
C9 N2 C10 105.5(5) . . ?
C9 N2 Cu1 122.6(4) . . ?
C10 N2 Cu1 130.8(4) . . ?
C4 C2 C3 117.3(4) . . ?
C4 C2 C1 119.6(4) . . ?
C3 C2 C1 123.1(4) . . ?
C3 C6 C7 120.5(5) . . ?
C5 C4 C2 121.4(5) . . ?
N2 C9 N1 112.2(5) . . ?
C7 C5 C4 120.2(5) . . ?
C1 C1 C2 122.8(3) 2_655 3_554 ?
C1 C1 C2 122.8(3) 2_655 . ?
C2 C1 C2 114.4(6) 3_554 . ?
C6 C3 C2 121.3(5) . . ?
C10 C8 N1 106.6(5) . . ?
C8 C10 N2 110.2(5) . . ?
Cu1 Cl1 Cu1 109.5 3 . ?
Cu1 Cl1 Cu1 109.5 3 4 ?
Cu1 Cl1 Cu1 109.5 . 4 ?
Cu1 Cl1 Cu1 109.5 3 2 ?
Cu1 Cl1 Cu1 109.5 . 2 ?
Cu1 Cl1 Cu1 109.5 4 2 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.340
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.100
