# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_l8_86cua

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C312 H176 N8 O148 Zn28'
_chemical_formula_weight         8234.97

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pm-3m

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

_cell_length_a                   32.366(5)
_cell_length_b                   32.366(5)
_cell_length_c                   32.366(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     33906(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    37820
_cell_measurement_theta_min      1.26
_cell_measurement_theta_max      20.04

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4128
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8832
_exptl_absorpt_correction_T_max  0.9275
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            93319
_diffrn_reflns_av_R_equivalents  0.4530
_diffrn_reflns_av_sigmaI/netI    0.1470
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         20.04
_reflns_number_total             3136
_reflns_number_gt                2019
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  WinGX

_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3136
_refine_ls_number_parameters     114
_refine_ls_number_restraints     232
_refine_ls_R_factor_all          0.3461
_refine_ls_R_factor_gt           0.2841
_refine_ls_wR_factor_ref         0.5560
_refine_ls_wR_factor_gt          0.5272
_refine_ls_goodness_of_fit_ref   1.693
_refine_ls_restrained_S_all      1.657
_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
Zn1 Zn 0.28530(10) 0.28530(10) 0.28530(10) 0.0520(16) Uani 1 6 d SD . .
Zn2 Zn 0.34927(10) 0.34927(10) 0.34927(10) 0.056(2) Uani 1 6 d SD . .
Zn3 Zn 0.5000 0.1389(2) 0.5000 0.0520(16) Uani 1 8 d SD . .
Zn4 Zn 0.5000 0.2301(2) 0.5000 0.0520(16) Uani 1 8 d SDU . .
O1 O 0.3203(6) 0.2529(9) 0.3203(6) 0.1503(13) Uani 1 2 d SDU . .
O2 O 0.3626(6) 0.2925(8) 0.3626(6) 0.1504(13) Uani 1 2 d SDU . .
O3 O 0.4588(5) 0.1491(7) 0.4588(5) 0.112(7) Uani 1 2 d SDU . .
O4 O 0.4574(5) 0.2199(7) 0.4574(5) 0.110(7) Uani 1 2 d SDU . .
C1 C 0.3667(7) 0.2218(6) 0.3667(7) 0.108(10) Uani 1 2 d SGDU . .
C2 C 0.3971(6) 0.2223(6) 0.3971(3) 0.084(9) Uani 1 2 d SGU . .
H2 H 0.4070 0.2474 0.4070 0.101 Uiso 1 2 calc SR . .
C3 C 0.4126(4) 0.1854(7) 0.4126(4) 0.109(10) Uani 1 2 d SGDU . .
C4 C 0.3978(8) 0.1479(6) 0.3978(8) 0.139(11) Uani 1 2 d SGDU . .
H4 H 0.4081 0.1232 0.4081 0.167 Uiso 1 2 calc SR . .
C5 C 0.3674(9) 0.1474(6) 0.3674(10) 0.175(10) Uani 1 2 d SGDU . .
C6 C 0.3519(7) 0.1843(8) 0.3519(6) 0.140(12) Uani 1 2 d SGDU . .
H6 H 0.3316 0.1840 0.3316 0.168 Uiso 1 2 calc SR . .
C7 C 0.3478(6) 0.2593(8) 0.3478(6) 0.1503(13) Uani 1 2 d SDU . .
C8 C 0.4450(4) 0.1838(8) 0.4450(4) 0.095(8) Uani 1 2 d SDU . .
C9 C 0.3520(9) 0.1087(9) 0.3520(9) 0.202(10) Uani 1 2 d SDU . .
C10 C 0.3408(9) 0.0757(7) 0.3408(9) 0.215(10) Uani 1 2 d SDU . .
C11 C 0.3259(9) 0.0367(5) 0.3259(9) 0.241(12) Uani 1 2 d SDU . .
C12 C 0.3415(11) 0.0000 0.3415(11) 0.255(18) Uani 1 4 d SDU . .
H12 H 0.3618 0.0000 0.3618 0.306 Uiso 1 4 calc SR . .
C13 C 0.2955(9) 0.0373(5) 0.2955(9) 0.282(16) Uani 1 2 d SDU . .
H13 H 0.2855 0.0623 0.2855 0.339 Uiso 1 2 calc SR . .
C14 C 0.2802(10) 0.0000 0.2802(10) 0.266(17) Uani 1 4 d SDU . .
H14 H 0.2598 0.0000 0.2598 0.319 Uiso 1 4 calc SR . .
O1W O 0.2499(3) 0.2499(3) 0.2499(3) 0.1504(13) Uani 1 6 d SD . .
O2W O 0.3849(3) 0.3849(3) 0.3849(3) 0.1504(13) Uani 1 6 d SD . .
O3W O 0.5000 0.0772(6) 0.5000 0.12(2) Uani 1 8 d SD . .
O4W O 0.5000 0.2918(6) 0.5000 0.186(15) Uani 1 8 d SDU . .


_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
Zn1 O1 1.91(3) . ?
Zn1 O1 1.91(3) 9 ?
Zn1 O1 1.91(3) 5 ?
Zn1 O1W 1.984(19) . ?
Zn2 O2 1.94(3) 9 ?
Zn2 O2 1.94(3) 5 ?
Zn2 O2 1.94(3) . ?
Zn2 O2W 2.000(19) . ?
Zn3 O3 1.92(2) 3_656 ?
Zn3 O3 1.92(2) 28_655 ?
Zn3 O3 1.92(2) 26_556 ?
Zn3 O3 1.92(2) . ?
Zn3 O3W 1.998(19) . ?
Zn3 Zn4 2.952(10) . ?
Zn4 O4 1.98(2) 28_655 ?
Zn4 O4 1.98(2) 26_556 ?
Zn4 O4 1.98(2) . ?
Zn4 O4 1.98(2) 3_656 ?
Zn4 O4W 1.998(19) . ?
O1 C7 1.277(17) . ?
O2 C7 1.270(17) . ?
O3 C8 1.288(17) . ?
O4 C8 1.298(17) . ?
C1 C2 1.390(15) . ?
C1 C6 1.390(8) . ?
C1 C7 1.492(18) . ?
C2 C3 1.3901 . ?
C3 C4 1.3900 . ?
C3 C8 1.485(17) . ?
C4 C5 1.3902 . ?
C5 C6 1.3901 . ?
C5 C9 1.437(15) . ?
C9 C10 1.185(17) . ?
C10 C11 1.433(16) . ?
C11 C12 1.387(13) . ?
C11 C13 1.392(17) . ?
C12 C11 1.387(13) 27 ?
C13 C14 1.396(13) . ?
C14 C13 1.396(13) 27 ?

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
O1 Zn1 O1 107.4(9) . 9 ?
O1 Zn1 O1 107.4(9) . 5 ?
O1 Zn1 O1 107.4(9) 9 5 ?
O1 Zn1 O1W 111.5(9) . . ?
O1 Zn1 O1W 111.5(9) 9 . ?
O1 Zn1 O1W 111.5(9) 5 . ?
O2 Zn2 O2 111.9(8) 9 5 ?
O2 Zn2 O2 111.9(8) 9 . ?
O2 Zn2 O2 111.9(8) 5 . ?
O2 Zn2 O2W 106.9(8) 9 . ?
O2 Zn2 O2W 106.9(8) 5 . ?
O2 Zn2 O2W 106.9(8) . . ?
O3 Zn3 O3 88.3(3) 3_656 28_655 ?
O3 Zn3 O3 88.3(3) 3_656 26_556 ?
O3 Zn3 O3 160.2(15) 28_655 26_556 ?
O3 Zn3 O3 160.2(15) 3_656 . ?
O3 Zn3 O3 88.3(3) 28_655 . ?
O3 Zn3 O3 88.3(3) 26_556 . ?
O3 Zn3 O3W 99.9(7) 3_656 . ?
O3 Zn3 O3W 99.9(7) 28_655 . ?
O3 Zn3 O3W 99.9(7) 26_556 . ?
O3 Zn3 O3W 99.9(7) . . ?
O3 Zn3 Zn4 80.1(7) 3_656 . ?
O3 Zn3 Zn4 80.1(7) 28_655 . ?
O3 Zn3 Zn4 80.1(7) 26_556 . ?
O3 Zn3 Zn4 80.1(7) . . ?
O3W Zn3 Zn4 180.000(1) . . ?
O4 Zn4 O4 160.8(14) 28_655 26_556 ?
O4 Zn4 O4 88.4(2) 28_655 . ?
O4 Zn4 O4 88.4(2) 26_556 . ?
O4 Zn4 O4 88.4(2) 28_655 3_656 ?
O4 Zn4 O4 88.4(2) 26_556 3_656 ?
O4 Zn4 O4 160.8(14) . 3_656 ?
O4 Zn4 O4W 99.6(7) 28_655 . ?
O4 Zn4 O4W 99.6(7) 26_556 . ?
O4 Zn4 O4W 99.6(7) . . ?
O4 Zn4 O4W 99.6(7) 3_656 . ?
O4 Zn4 Zn3 80.4(7) 28_655 . ?
O4 Zn4 Zn3 80.4(7) 26_556 . ?
O4 Zn4 Zn3 80.4(7) . . ?
O4 Zn4 Zn3 80.4(7) 3_656 . ?
O4W Zn4 Zn3 180.000(2) . . ?
C7 O1 Zn1 137(2) . . ?
C7 O2 Zn2 129(2) . . ?
C8 O3 Zn3 129.1(19) . . ?
C8 O4 Zn4 125.4(17) . . ?
C2 C1 C6 120.0(6) . . ?
C2 C1 C7 124.8(19) . . ?
C6 C1 C7 115(2) . . ?
C1 C2 C3 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 C8 117.3(17) . . ?
C2 C3 C8 122.7(17) . . ?
C3 C4 C5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 C9 120.0(19) . . ?
C6 C5 C9 120.0(19) . . ?
C5 C6 C1 120.0(5) . . ?
O2 C7 O1 132(3) . . ?
O2 C7 C1 112(2) . . ?
O1 C7 C1 116(2) . . ?
O3 C8 O4 125(2) . . ?
O3 C8 C3 121(2) . . ?
O4 C8 C3 114(2) . . ?
C10 C9 C5 176(5) . . ?
C9 C10 C11 177(5) . . ?
C12 C11 C13 121.7(18) . . ?
C12 C11 C10 120.7(19) . . ?
C13 C11 C10 117.6(18) . . ?
C11 C12 C11 118(3) 27 . ?
C11 C13 C14 119.4(19) . . ?
C13 C14 C13 120(3) . 27 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        20.04
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.473
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.160

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.004 -0.010 -0.005 28365 8581 ' '
_platon_squeeze_details          ?
_database_code_depnum_ccdc_archive 'CCDC 969629'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_p7_60cu

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C288 H200 N32 O172 Zn28'
_chemical_formula_weight         8691.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   Pm-3

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

_cell_length_a                   31.102(4)
_cell_length_b                   31.102(4)
_cell_length_c                   31.102(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     30086(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    124327
_cell_measurement_theta_min      1.30
_cell_measurement_theta_max      19.54

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4368
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_type   Multi-scans
_exptl_absorpt_correction_T_min  0.8462
_exptl_absorpt_correction_T_max  0.9186
_exptl_absorpt_process_details   'HKL2000 Scalepack'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.00000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18250
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.30
_diffrn_reflns_theta_max         19.54
_reflns_number_total             1748
_reflns_number_gt                1134
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL2000
_computing_data_reduction        HKL2000
_computing_structure_solution    'Bruker SHELXTL-XS'
_computing_structure_refinement  'Bruker SHELXTL-XL'
_computing_molecular_graphics    'Diamond 3'
_computing_publication_material  WinGX

_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1748
_refine_ls_number_parameters     176
_refine_ls_number_restraints     133
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.1101
_refine_ls_wR_factor_ref         0.2876
_refine_ls_wR_factor_gt          0.2660
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.174
_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
Zn1 Zn 0.5000 0.5000 0.12743(14) 0.229(3) Uani 1 4 d SD . .
Zn2 Zn 0.5000 0.5000 0.22334(17) 0.216(3) Uani 1 4 d SD . .
Zn3 Zn 0.34329(11) 0.34329(11) 0.34329(11) 0.250(3) Uani 1 3 d SD . .
Zn4 Zn 0.27804(11) 0.27804(11) 0.27804(11) 0.301(4) Uani 1 3 d SD . .
O1 O 0.4572(6) 0.4581(5) 0.1403(6) 0.336(9) Uani 1 1 d D . .
O2 O 0.4562(5) 0.4569(5) 0.2113(4) 0.286(9) Uani 1 1 d D . .
O3 O 0.3581(5) 0.3585(5) 0.2858(5) 0.264(8) Uani 1 1 d D . .
O4 O 0.3151(5) 0.3178(5) 0.2473(5) 0.324(8) Uani 1 1 d D . .
O5 O 0.3218(11) 0.2767(12) 0.1038(10) 0.81(4) Uani 1 1 d D . .
N1 N 0.3854(5) 0.3101(5) 0.1034(5) 0.59(3) Uani 1 1 d D . .
H1 H 0.4101 0.3061 0.0901 0.707 Uiso 1 1 calc R . .
C1 C 0.4191(5) 0.4034(5) 0.1718(5) 0.53(4) Uani 1 1 d RDU . .
C2 C 0.3957(5) 0.3969(5) 0.2093(5) 0.331(18) Uani 1 1 d RDU . .
H2 H 0.3969 0.4175 0.2319 0.398 Uiso 1 1 calc R . .
C3 C 0.3705(5) 0.3603(5) 0.2139(5) 0.41(3) Uani 1 1 d RDU . .
C4 C 0.3687(5) 0.3302(5) 0.1809(5) 0.65(5) Uani 1 1 d RDU . .
H4 H 0.3514 0.3052 0.1840 0.776 Uiso 1 1 calc R . .
C5 C 0.3921(5) 0.3367(5) 0.1434(5) 0.59(4) Uani 1 1 d RDU . .
C6 C 0.4173(5) 0.3733(5) 0.1389(5) 0.67(5) Uani 1 1 d RDU . .
H6 H 0.4334 0.3777 0.1133 0.800 Uiso 1 1 calc R . .
C7 C 0.4447(6) 0.4405(6) 0.1758(7) 0.269(13) Uani 1 1 d DU . .
C8 C 0.3470(6) 0.3448(6) 0.2488(7) 0.281(15) Uani 1 1 d DU . .
C9 C 0.3540(11) 0.2909(16) 0.0820(9) 0.89(8) Uani 1 1 d DU . .
C10 C 0.3568(16) 0.2955(13) 0.0000 0.61(5) Uani 1 2 d SDU . .
H10 H 0.3499 0.3253 0.0000 0.728 Uiso 1 2 calc SR . .
C11 C 0.3619(9) 0.2735(9) 0.0388(5) 0.78(6) Uani 1 1 d DU . .
C12 C 0.3730(13) 0.2304(10) 0.0387(6) 0.72(5) Uani 1 1 d DU . .
H12 H 0.3767 0.2156 0.0651 0.859 Uiso 1 1 calc R . .
C13 C 0.3788(18) 0.2087(13) 0.0000 0.63(5) Uani 1 2 d SDU . .
H13 H 0.3867 0.1791 0.0000 0.751 Uiso 1 2 calc SR . .
O1W O 0.5000 0.5000 0.0636(6) 0.326(13) Uani 1 4 d SD . .
O2W O 0.5000 0.5000 0.2898(5) 0.230(9) Uani 1 4 d SD . .
O3W O 0.3804(3) 0.3804(3) 0.3804(3) 0.290(10) Uani 1 3 d SD . .
O4W O 0.2409(4) 0.2409(4) 0.2409(4) 0.61(3) Uani 1 3 d SD . .


_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
Zn1 O1 1.907(15) 2_665 ?
Zn1 O1 1.907(15) 15_565 ?
Zn1 O1 1.907(15) 16_655 ?
Zn1 O1 1.908(15) . ?
Zn1 O1W 1.984(17) . ?
Zn1 Zn2 2.983(7) . ?
Zn2 O2 1.947(15) . ?
Zn2 O2 1.947(15) 16_655 ?
Zn2 O2 1.947(15) 2_665 ?
Zn2 O2 1.947(15) 15_565 ?
Zn2 O2W 2.067(15) . ?
Zn3 O3 1.907(14) . ?
Zn3 O3 1.907(14) 9 ?
Zn3 O3 1.907(14) 5 ?
Zn3 O3W 2.000(16) . ?
Zn4 O4 1.944(14) 5 ?
Zn4 O4 1.944(14) . ?
Zn4 O4 1.944(14) 9 ?
Zn4 O4W 2.00(2) . ?
O1 C7 1.292(15) . ?
O2 C7 1.269(16) . ?
O3 C8 1.273(16) . ?
O4 C8 1.298(15) . ?
O5 C9 1.29(2) . ?
N1 C9 1.32(2) . ?
N1 C5 1.5084 . ?
C1 C2 1.3898 . ?
C1 C6 1.3898 . ?
C1 C7 1.406(16) . ?
C2 C3 1.3898 . ?
C3 C4 1.3898 . ?
C3 C8 1.396(16) . ?
C4 C5 1.3898 . ?
C5 C6 1.3898 . ?
C9 C11 1.467(19) . ?
C10 C11 1.398(15) 14 ?
C10 C11 1.398(15) . ?
C11 C12 1.38(2) . ?
C12 C13 1.392(15) . ?
C13 C12 1.392(15) 14 ?

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
O1 Zn1 O1 88.6(12) 2_665 15_565 ?
O1 Zn1 O1 86.3(11) 2_665 16_655 ?
O1 Zn1 O1 155.7(10) 15_565 16_655 ?
O1 Zn1 O1 155.7(10) 2_665 . ?
O1 Zn1 O1 86.3(11) 15_565 . ?
O1 Zn1 O1 88.6(12) 16_655 . ?
O1 Zn1 O1W 102.1(5) 2_665 . ?
O1 Zn1 O1W 102.1(5) 15_565 . ?
O1 Zn1 O1W 102.1(5) 16_655 . ?
O1 Zn1 O1W 102.2(5) . . ?
O1 Zn1 Zn2 77.9(5) 2_665 . ?
O1 Zn1 Zn2 77.9(5) 15_565 . ?
O1 Zn1 Zn2 77.9(5) 16_655 . ?
O1 Zn1 Zn2 77.8(5) . . ?
O1W Zn1 Zn2 180.000(1) . . ?
O2 Zn2 O2 88.7(9) . 16_655 ?
O2 Zn2 O2 157.9(9) . 2_665 ?
O2 Zn2 O2 87.0(9) 16_655 2_665 ?
O2 Zn2 O2 87.0(9) . 15_565 ?
O2 Zn2 O2 157.8(9) 16_655 15_565 ?
O2 Zn2 O2 88.7(9) 2_665 15_565 ?
O2 Zn2 O2W 101.1(4) . . ?
O2 Zn2 O2W 101.1(4) 16_655 . ?
O2 Zn2 O2W 101.1(4) 2_665 . ?
O2 Zn2 O2W 101.1(4) 15_565 . ?
O2 Zn2 Zn1 78.9(4) . . ?
O2 Zn2 Zn1 78.9(4) 16_655 . ?
O2 Zn2 Zn1 78.9(4) 2_665 . ?
O2 Zn2 Zn1 78.9(4) 15_565 . ?
O2W Zn2 Zn1 180.000(1) . . ?
O3 Zn3 O3 113.5(4) . 9 ?
O3 Zn3 O3 113.5(4) . 5 ?
O3 Zn3 O3 113.5(4) 9 5 ?
O3 Zn3 O3W 105.0(5) . . ?
O3 Zn3 O3W 105.0(5) 9 . ?
O3 Zn3 O3W 105.0(5) 5 . ?
O4 Zn4 O4 103.2(6) 5 . ?
O4 Zn4 O4 103.2(6) 5 9 ?
O4 Zn4 O4 103.2(6) . 9 ?
O4 Zn4 O4W 115.2(5) 5 . ?
O4 Zn4 O4W 115.2(5) . . ?
O4 Zn4 O4W 115.2(5) 9 . ?
C7 O1 Zn1 132.8(14) . . ?
C7 O2 Zn2 130.0(14) . . ?
C8 O3 Zn3 134.3(15) . . ?
C8 O4 Zn4 147.7(15) . . ?
C9 N1 C5 139.8(14) . . ?
C2 C1 C6 120.0 . . ?
C2 C1 C7 109.9(10) . . ?
C6 C1 C7 129.9(10) . . ?
C3 C2 C1 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 C8 131.1(10) . . ?
C4 C3 C8 108.7(10) . . ?
C5 C4 C3 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 N1 122.7 . . ?
C6 C5 N1 116.3 . . ?
C5 C6 C1 120.0 . . ?
O2 C7 O1 119.2(19) . . ?
O2 C7 C1 124.6(17) . . ?
O1 C7 C1 116.2(17) . . ?
O3 C8 O4 117(2) . . ?
O3 C8 C3 116.4(17) . . ?
O4 C8 C3 126.4(18) . . ?
O5 C9 N1 118(2) . . ?
O5 C9 C11 119(2) . . ?
N1 C9 C11 120(2) . . ?
C11 C10 C11 120(3) 14 . ?
C12 C11 C10 120(2) . . ?
C12 C11 C9 114(3) . . ?
C10 C11 C9 126(3) . . ?
C11 C12 C13 120(2) . . ?
C12 C13 C12 120(3) . 14 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        19.54
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.056

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.004 -0.017 -0.005 24176 5275 ' '
_platon_squeeze_details          ?
_database_code_depnum_ccdc_archive 'CCDC 969630'
