# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_a30530b
_database_code_depnum_ccdc_archive 'CCDC 1032538'
_audit_update_record             
;
2015-02-02 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H28 N2 O18 Zn3, 2(C3 H7 N O)'
_chemical_formula_sum            'C44 H42 N4 O20 Zn3'
_chemical_formula_weight         1142.92

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'
Zn Zn 0.2839 1.4301 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.646(6)
_cell_length_b                   18.345(7)
_cell_length_c                   16.309(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.893(4)
_cell_angle_gamma                90
_cell_volume                     4712(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    815
_cell_measurement_theta_min      2.583
_cell_measurement_theta_max      25.134

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_F_000             2336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.599
_shelx_estimated_absorpt_T_min   0.645
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.829628
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7790
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.704
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measured_fraction_theta_full 0.892
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_Laue_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_point_group_measured_fraction_full 0.892
_reflns_number_total             3797
_reflns_number_gt                2654
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0821P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3797
_refine_ls_number_parameters     326
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0473
_refine_ls_wR_factor_ref         0.1342
_refine_ls_wR_factor_gt          0.1199
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      0.954
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.05950(3) 0.13772(3) 0.36451(4) 0.0254(2) Uani 1 1 d . . . . .
Zn2 Zn 0.2500 0.2500 0.5000 0.0284(2) Uani 1 2 d S . P . .
O1 O 0.0969(2) 0.09731(19) 0.4812(2) 0.0373(9) Uani 1 1 d . . . . .
O2 O 0.2264(2) 0.14091(17) 0.5046(2) 0.0324(8) Uani 1 1 d . . . . .
O3 O 0.5105(2) 0.26561(19) 0.8497(3) 0.0496(11) Uani 1 1 d . . . . .
O4 O 0.6217(3) 0.2248(2) 0.9492(4) 0.100(2) Uani 1 1 d . . . . .
O5 O 0.6587(3) -0.0404(2) 0.9950(3) 0.0732(15) Uani 1 1 d . . . . .
H5B H 0.6859 -0.0785 1.0063 0.110 Uiso 1 1 calc R U . . .
O6 O 0.5535(3) -0.1161(2) 0.9272(3) 0.0693(14) Uani 1 1 d . . . . .
O7 O 0.1358(2) -0.09608(19) 0.8085(2) 0.0356(9) Uani 1 1 d . . . . .
O8 O 0.0436(2) -0.0770(2) 0.6766(2) 0.0468(11) Uani 1 1 d . . . . .
C1 C 0.1745(3) 0.1052(2) 0.5274(3) 0.0284(12) Uani 1 1 d . . . . .
C2 C 0.2015(3) 0.0682(3) 0.6141(3) 0.0300(12) Uani 1 1 d . . . . .
C3 C 0.2816(3) 0.0820(3) 0.6721(3) 0.0351(13) Uani 1 1 d . . . . .
H3A H 0.3174 0.1147 0.6574 0.042 Uiso 1 1 calc R U . . .
C4 C 0.3092(3) 0.0470(3) 0.7533(3) 0.0289(12) Uani 1 1 d . . . . .
C5 C 0.2536(3) -0.0025(3) 0.7741(3) 0.0360(14) Uani 1 1 d . . . . .
H5A H 0.2702 -0.0260 0.8275 0.043 Uiso 1 1 calc R U . . .
C6 C 0.1737(3) -0.0158(3) 0.7143(3) 0.0285(12) Uani 1 1 d . . . . .
C7 C 0.1488(3) 0.0188(3) 0.6342(3) 0.0376(14) Uani 1 1 d . . . . .
H7A H 0.0961 0.0085 0.5940 0.045 Uiso 1 1 calc R U . . .
C8 C 0.1128(3) -0.0668(3) 0.7353(3) 0.0337(13) Uani 1 1 d . . . . .
C9 C 0.3974(3) 0.0593(3) 0.8126(3) 0.0369(14) Uani 1 1 d . . . . .
C10 C 0.4338(3) 0.1285(3) 0.8240(3) 0.0303(12) Uani 1 1 d . . . . .
H10A H 0.4033 0.1676 0.7927 0.036 Uiso 1 1 calc R U . . .
C11 C 0.5151(3) 0.1400(3) 0.8813(3) 0.0302(12) Uani 1 1 d . . . . .
C12 C 0.5634(3) 0.0811(3) 0.9232(3) 0.0371(14) Uani 1 1 d . . . . .
H12A H 0.6180 0.0884 0.9614 0.045 Uiso 1 1 calc R U . . .
C13 C 0.5302(3) 0.0114(3) 0.9079(3) 0.0347(13) Uani 1 1 d . . . . .
C14 C 0.4473(3) 0.0017(3) 0.8553(4) 0.0371(14) Uani 1 1 d . . . . .
H14A H 0.4242 -0.0450 0.8484 0.045 Uiso 1 1 calc R U . . .
C15 C 0.5528(3) 0.2156(3) 0.8938(4) 0.0384(14) Uani 1 1 d . . . . .
C16 C 0.5812(3) -0.0545(3) 0.9444(4) 0.0440(15) Uani 1 1 d . . . . .
N1 N 0.2009(4) 0.2941(3) 0.7362(4) 0.0712(19) Uani 1 1 d . . . . .
O9 O 0.2488(4) 0.2615(3) 0.6297(4) 0.0818(17) Uani 1 1 d . . . . .
C17 C 0.1968(5) 0.2862(4) 0.6494(9) 0.111(5) Uani 1 1 d . . . . .
H17A H 0.1484 0.3024 0.6063 0.133 Uiso 1 1 calc R U . . .
C18 C 0.2762(7) 0.2826(6) 0.8069(6) 0.123(4) Uani 1 1 d . . . . .
H18A H 0.2753 0.2347 0.8301 0.184 Uiso 1 1 calc R U . . .
H18B H 0.2798 0.3183 0.8510 0.184 Uiso 1 1 calc R U . . .
H18C H 0.3246 0.2872 0.7874 0.184 Uiso 1 1 calc R U . . .
C19 C 0.1278(6) 0.3208(6) 0.7567(7) 0.134(4) Uani 1 1 d . . . . .
H19A H 0.1443 0.3616 0.7955 0.201 Uiso 1 1 calc R U . . .
H19B H 0.1059 0.2828 0.7839 0.201 Uiso 1 1 calc R U . . .
H19C H 0.0847 0.3359 0.7044 0.201 Uiso 1 1 calc R U . . .
N2 N 0.8987(5) 0.8499(4) 0.0768(5) 0.089(2) Uani 1 1 d . . . . .
O10 O 0.7582(5) 0.8451(4) 0.0399(6) 0.162(4) Uani 1 1 d . . . . .
C20 C 0.8305(9) 0.8132(8) 0.0447(8) 0.141(5) Uani 1 1 d . . . . .
H20A H 0.8318 0.7656 0.0256 0.169 Uiso 1 1 calc R U . . .
C21 C 0.9651(12) 0.8086(10) 0.0733(14) 0.318(14) Uani 1 1 d . . . . .
H21A H 0.9463 0.7595 0.0582 0.477 Uiso 1 1 calc R U . . .
H21B H 1.0086 0.8090 0.1289 0.477 Uiso 1 1 calc R U . . .
H21C H 0.9873 0.8281 0.0304 0.477 Uiso 1 1 calc R U . . .
C22 C 0.9042(12) 0.9221(6) 0.0966(11) 0.255(9) Uani 1 1 d . . . . .
H22A H 0.8729 0.9497 0.0463 0.383 Uiso 1 1 calc R U . . .
H22B H 0.9627 0.9369 0.1151 0.383 Uiso 1 1 calc R U . . .
H22C H 0.8809 0.9308 0.1424 0.383 Uiso 1 1 calc R U . . .


_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 O3 1.934(3) 8_455 ?
Zn1 O7 1.945(3) 6 ?
Zn1 O1 1.947(3) . ?
Zn1 O8 1.972(3) 5_556 ?
Zn2 O2 2.045(3) 7_556 ?
Zn2 O2 2.045(3) . ?
Zn2 O4 2.077(4) 8_455 ?
Zn2 O4 2.077(4) 2_656 ?
Zn2 O9 2.133(6) 7_556 ?
Zn2 O9 2.133(6) . ?
O1 C1 1.276(5) . ?
O2 C1 1.233(6) . ?
O3 C15 1.235(6) . ?
O3 Zn1 1.934(3) 8_556 ?
O4 C15 1.221(6) . ?
O4 Zn2 2.077(4) 2_656 ?
O5 C16 1.313(7) . ?
O6 C16 1.220(6) . ?
O7 C8 1.250(6) . ?
O7 Zn1 1.945(3) 6_556 ?
O8 C8 1.251(6) . ?
O8 Zn1 1.972(3) 5_556 ?
C1 C2 1.501(7) . ?
C2 C7 1.373(7) . ?
C2 C3 1.386(6) . ?
C3 C4 1.408(7) . ?
C4 C5 1.414(7) . ?
C4 C9 1.490(6) . ?
C5 C6 1.392(6) . ?
C6 C7 1.389(7) . ?
C6 C8 1.499(7) . ?
C9 C14 1.385(7) . ?
C9 C10 1.393(6) . ?
C10 C11 1.389(7) . ?
C11 C12 1.388(7) . ?
C11 C15 1.509(7) . ?
C12 C13 1.382(7) . ?
C13 C14 1.381(7) . ?
C13 C16 1.486(7) . ?
N1 C17 1.402(13) . ?
N1 C18 1.417(10) . ?
N1 C19 1.449(10) . ?
O9 C17 1.112(10) . ?
N2 C20 1.277(13) . ?
N2 C21 1.356(13) . ?
N2 C22 1.359(12) . ?
O10 C20 1.318(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
O3 Zn1 O7 127.92(18) 8_455 6 ?
O3 Zn1 O1 117.37(17) 8_455 . ?
O7 Zn1 O1 105.02(15) 6 . ?
O3 Zn1 O8 100.93(17) 8_455 5_556 ?
O7 Zn1 O8 104.31(16) 6 5_556 ?
O1 Zn1 O8 94.86(14) . 5_556 ?
O2 Zn2 O2 180.0 7_556 . ?
O2 Zn2 O4 87.26(15) 7_556 8_455 ?
O2 Zn2 O4 92.74(15) . 8_455 ?
O2 Zn2 O4 92.74(15) 7_556 2_656 ?
O2 Zn2 O4 87.26(15) . 2_656 ?
O4 Zn2 O4 180.0 8_455 2_656 ?
O2 Zn2 O9 89.79(16) 7_556 7_556 ?
O2 Zn2 O9 90.21(16) . 7_556 ?
O4 Zn2 O9 88.0(3) 8_455 7_556 ?
O4 Zn2 O9 92.0(3) 2_656 7_556 ?
O2 Zn2 O9 90.21(16) 7_556 . ?
O2 Zn2 O9 89.79(16) . . ?
O4 Zn2 O9 92.0(3) 8_455 . ?
O4 Zn2 O9 88.0(3) 2_656 . ?
O9 Zn2 O9 180.0(4) 7_556 . ?
C1 O1 Zn1 118.4(3) . . ?
C1 O2 Zn2 133.8(3) . . ?
C15 O3 Zn1 118.0(3) . 8_556 ?
C15 O4 Zn2 157.6(6) . 2_656 ?
C8 O7 Zn1 124.9(3) . 6_556 ?
C8 O8 Zn1 146.0(4) . 5_556 ?
O2 C1 O1 123.8(5) . . ?
O2 C1 C2 119.9(4) . . ?
O1 C1 C2 116.2(4) . . ?
C7 C2 C3 120.3(5) . . ?
C7 C2 C1 120.3(4) . . ?
C3 C2 C1 119.3(4) . . ?
C2 C3 C4 120.5(5) . . ?
C3 C4 C5 118.6(4) . . ?
C3 C4 C9 119.5(4) . . ?
C5 C4 C9 121.7(4) . . ?
C6 C5 C4 119.7(5) . . ?
C7 C6 C5 120.3(4) . . ?
C7 C6 C8 118.9(4) . . ?
C5 C6 C8 120.9(4) . . ?
C2 C7 C6 120.5(4) . . ?
O7 C8 O8 126.0(5) . . ?
O7 C8 C6 117.7(4) . . ?
O8 C8 C6 116.2(5) . . ?
C14 C9 C10 117.6(4) . . ?
C14 C9 C4 121.0(4) . . ?
C10 C9 C4 121.3(4) . . ?
C11 C10 C9 121.0(4) . . ?
C12 C11 C10 119.7(4) . . ?
C12 C11 C15 120.0(4) . . ?
C10 C11 C15 120.2(4) . . ?
C13 C12 C11 119.8(5) . . ?
C14 C13 C12 119.5(5) . . ?
C14 C13 C16 118.1(5) . . ?
C12 C13 C16 122.4(5) . . ?
C13 C14 C9 122.0(4) . . ?
O4 C15 O3 123.4(5) . . ?
O4 C15 C11 118.5(5) . . ?
O3 C15 C11 118.1(4) . . ?
O6 C16 O5 123.2(5) . . ?
O6 C16 C13 122.5(5) . . ?
O5 C16 C13 114.2(5) . . ?
C17 N1 C18 123.2(8) . . ?
C17 N1 C19 119.9(8) . . ?
C18 N1 C19 116.7(8) . . ?
C17 O9 Zn2 125.8(9) . . ?
O9 C17 N1 123.0(10) . . ?
C20 N2 C21 108.4(13) . . ?
C20 N2 C22 126.4(12) . . ?
C21 N2 C22 124.1(14) . . ?
N2 C20 O10 117.6(13) . . ?

_refine_diff_density_max         0.885
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.097

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_a30530c
_database_code_depnum_ccdc_archive 'CCDC 1032539'
_audit_update_record             
;
2015-02-02 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H36 N2 O25 Zn5'
_chemical_formula_weight         1415.68

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   12.145(11)
_cell_length_b                   30.72(3)
_cell_length_c                   22.75(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.000(12)
_cell_angle_gamma                90
_cell_volume                     8468(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    987
_cell_measurement_theta_min      2.463
_cell_measurement_theta_max      27.054

_exptl_crystal_description       block
_exptl_crystal_colour            paleyellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_F_000             2848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.454
_shelx_estimated_absorpt_T_min   0.670
_shelx_estimated_absorpt_T_max   0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.763720
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20605
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.601
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             7520
_reflns_number_gt                5465
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
; 
 w=1/[σ²(Fo²)+(0.1518P)²+0.2588P] 
 where P=(Fo²+2Fc²)/3 
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7520
_refine_ls_number_parameters     384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.2021
_refine_ls_wR_factor_gt          0.1885
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_restrained_S_all      0.934
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.31427(4) 0.13252(2) 0.48747(2) 0.02528(19) Uani 1 1 d . . . . .
Zn2 Zn 0.25880(4) 0.08310(2) 0.34284(2) 0.02607(19) Uani 1 1 d . . . . .
Zn3 Zn 0.0000 0.03794(3) 0.2500 0.0446(3) Uani 1 2 d S T P . .
O1 O 0.2606(3) 0.17288(12) 0.42348(15) 0.0431(10) Uani 1 1 d . . . . .
O2 O 0.1756(3) 0.13581(12) 0.34893(18) 0.0423(10) Uani 1 1 d . . . . .
O3 O 0.1594(4) 0.32299(13) 0.45454(16) 0.0528(12) Uani 1 1 d . . . . .
O4 O 0.0691(6) 0.36042(16) 0.3853(3) 0.104(3) Uani 1 1 d . . . . .
O5 O 0.2246(3) 0.02983(12) 0.38104(18) 0.0430(10) Uani 1 1 d . . . . .
O6 O 0.0523(3) 0.03438(15) 0.34154(18) 0.0533(12) Uani 1 1 d . . . . .
O7 O -0.2375(4) -0.0606(2) 0.4270(3) 0.094(2) Uani 1 1 d . . . . .
O8 O -0.1837(3) -0.09881(16) 0.50493(19) 0.0524(11) Uani 1 1 d . . . . .
O9 O 0.1223(4) -0.0766(2) 0.7285(2) 0.050(2) Uani 0.767(13) 1 d . . P A 2
O9' O 0.1633(16) -0.0393(7) 0.7282(8) 0.051(7) Uiso 0.233(13) 1 d . . P A 1
O10 O 0.2979(3) -0.07964(14) 0.76138(16) 0.0476(11) Uani 1 1 d . . . . .
O11 O 0.5890(3) -0.09635(16) 0.62561(17) 0.0513(11) Uani 1 1 d . . . . .
O12 O 0.5460(3) -0.10612(13) 0.53066(15) 0.0382(9) Uani 1 1 d . . . . .
O13 O 0.0000 -0.0311(6) 0.2500 0.107(7) Uani 0.5 2 d S T P B 2
O13' O -0.0930(17) -0.0231(6) 0.2602(9) 0.060(5) Uiso 0.25 1 d . . P B 1
C1 C 0.1977(4) 0.17015(17) 0.3780(2) 0.0332(12) Uani 1 1 d . . . . .
C2 C 0.1430(4) 0.21065(17) 0.3551(2) 0.0339(12) Uani 1 1 d . . . . .
C3 C 0.1513(5) 0.24828(17) 0.3887(2) 0.0375(13) Uani 1 1 d . . . . .
H3A H 0.1902 0.2479 0.4254 0.045 Uiso 1 1 calc R U . . .
C4 C 0.1019(5) 0.28647(17) 0.3679(2) 0.0393(13) Uani 1 1 d . . . . .
C5 C 0.0417(5) 0.28636(18) 0.3136(2) 0.0458(16) Uani 1 1 d . . . . .
H5A H 0.0070 0.3118 0.3000 0.055 Uiso 1 1 calc R U . . .
C6 C 0.0326(5) 0.24882(18) 0.2793(2) 0.0412(14) Uani 1 1 d . . . . .
C7 C 0.0831(5) 0.21121(17) 0.3008(2) 0.0378(13) Uani 1 1 d . . . . .
H7A H 0.0769 0.1858 0.2786 0.045 Uiso 1 1 calc R U . . .
C8 C 0.1097(6) 0.3270(2) 0.4045(3) 0.0494(16) Uani 1 1 d . . . . .
C9 C 0.1225(5) 0.01769(18) 0.3766(2) 0.0351(12) Uani 1 1 d . . . . .
C10 C 0.0908(4) -0.01554(17) 0.4190(2) 0.0308(11) Uani 1 1 d . . . . .
C11 C -0.0168(4) -0.02962(17) 0.4188(2) 0.0322(12) Uani 1 1 d . . . . .
H11A H -0.0688 -0.0198 0.3899 0.039 Uiso 1 1 calc R U . . .
C12 C -0.0484(4) -0.05853(18) 0.4619(2) 0.0333(12) Uani 1 1 d . . . . .
C13 C 0.0285(4) -0.07265(18) 0.5054(2) 0.0319(12) Uani 1 1 d . . . . .
H13 H 0.0073 -0.0917 0.5343 0.038 Uiso 1 1 calc R U . . .
C14 C 0.1383(4) -0.05835(17) 0.5063(2) 0.0288(11) Uani 1 1 d . . . . .
C15 C 0.1680(4) -0.03049(16) 0.4627(2) 0.0292(11) Uani 1 1 d . . . . .
H15A H 0.2410 -0.0214 0.4623 0.035 Uiso 1 1 calc R U . . .
C16 C 0.2186(4) -0.07089(17) 0.5554(2) 0.0300(11) Uani 1 1 d . . . . .
C17 C 0.1858(5) -0.0703(2) 0.6128(2) 0.0406(14) Uani 1 1 d . . . . .
H17A H 0.1126 -0.0645 0.6196 0.049 Uiso 1 1 calc R U . . .
C18 C 0.2624(5) -0.0784(2) 0.6603(2) 0.0406(14) Uani 1 1 d . . . . .
C19 C 0.3731(4) -0.08668(18) 0.6501(2) 0.0344(12) Uani 1 1 d . . . . .
H19A H 0.4249 -0.0910 0.6816 0.041 Uiso 1 1 calc R U . . .
C20 C 0.4047(4) -0.08849(16) 0.5924(2) 0.0272(11) Uani 1 1 d . . . . .
C21 C 0.3279(4) -0.08096(16) 0.5453(2) 0.0298(11) Uani 1 1 d . . . . .
H21A H 0.3494 -0.0826 0.5070 0.036 Uiso 1 1 calc R U . . .
C22 C -0.1666(5) -0.0737(2) 0.4636(3) 0.0422(14) Uani 1 1 d . . . . .
C23 C 0.2261(5) -0.0755(2) 0.7215(2) 0.0499(17) Uani 1 1 d . . . . .
C24 C 0.5223(4) -0.09766(17) 0.5822(2) 0.0301(11) Uani 1 1 d . . . . .
N1 N 0.4502(14) 0.0541(4) 0.6191(6) 0.190(7) Uani 1 1 d . . . . .
H1A H 0.3892 0.0728 0.6055 0.228 Uiso 1 1 calc R U . . .
H1B H 0.5115 0.0723 0.6338 0.228 Uiso 1 1 calc R U . . .
C25 C 0.4838(12) 0.0251(5) 0.5703(8) 0.167(7) Uani 1 1 d . . . . .
H25A H 0.5070 0.0426 0.5385 0.251 Uiso 1 1 calc R U . . .
H25D H 0.4223 0.0074 0.5565 0.251 Uiso 1 1 calc R U . . .
H25B H 0.5437 0.0068 0.5848 0.251 Uiso 1 1 calc R U . . .
C26 C 0.416(2) 0.0234(10) 0.6663(11) 0.326(15) Uiso 1 1 d . . . . .
H26D H 0.3933 0.0399 0.6992 0.490 Uiso 1 1 calc R U . . .
H26A H 0.4775 0.0052 0.6790 0.490 Uiso 1 1 calc R U . . .
H26B H 0.3561 0.0056 0.6507 0.490 Uiso 1 1 calc R U . . .


_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 O3 1.911(4) 7_556 ?
Zn1 O8 1.911(4) 5_556 ?
Zn1 O12 1.951(4) 5_656 ?
Zn1 O1 1.987(4) . ?
Zn2 O5 1.912(4) . ?
Zn2 O2 1.919(4) . ?
Zn2 O10 1.948(4) 6 ?
Zn2 O11 1.978(4) 5_656 ?
Zn3 O9 1.989(5) 6 ?
Zn3 O9 1.989(5) 5_556 ?
Zn3 O9' 2.08(2) 6 ?
Zn3 O9' 2.08(2) 5_556 ?
Zn3 O13 2.121(19) . ?
Zn3 O6 2.138(4) 2 ?
Zn3 O6 2.138(4) . ?
Zn3 O13' 2.210(19) . ?
Zn3 O13' 2.210(19) 2 ?
O1 C1 1.247(6) . ?
O2 C1 1.263(6) . ?
O3 C8 1.257(7) . ?
O3 Zn1 1.911(4) 7_556 ?
O4 C8 1.207(7) . ?
O5 C9 1.292(7) . ?
O6 C9 1.238(6) . ?
O7 C22 1.223(7) . ?
O8 C22 1.246(7) . ?
O8 Zn1 1.912(4) 5_556 ?
O9 C23 1.281(8) . ?
O9 Zn3 1.989(5) 5_556 ?
O9' C23 1.36(2) . ?
O9' Zn3 2.078(19) 5_556 ?
O10 C23 1.221(7) . ?
O10 Zn2 1.948(4) 6_556 ?
O11 C24 1.233(6) . ?
O11 Zn2 1.978(4) 5_656 ?
O12 C24 1.255(6) . ?
O12 Zn1 1.951(4) 5_656 ?
C1 C2 1.487(7) . ?
C2 C3 1.386(7) . ?
C2 C7 1.390(7) . ?
C3 C4 1.386(7) . ?
C4 C5 1.391(7) . ?
C4 C8 1.498(8) . ?
C5 C6 1.393(8) . ?
C6 C7 1.382(7) . ?
C6 C6 1.501(10) 2 ?
C9 C10 1.474(7) . ?
C10 C11 1.376(7) . ?
C10 C15 1.396(7) . ?
C11 C12 1.395(7) . ?
C12 C13 1.384(7) . ?
C12 C22 1.512(7) . ?
C13 C14 1.402(7) . ?
C14 C15 1.378(7) . ?
C14 C16 1.481(6) . ?
C16 C17 1.392(7) . ?
C16 C21 1.398(7) . ?
C17 C18 1.398(7) . ?
C18 C19 1.404(8) . ?
C18 C23 1.493(8) . ?
C19 C20 1.393(7) . ?
C20 C21 1.390(7) . ?
C20 C24 1.490(7) . ?
N1 C25 1.502(17) . ?
N1 C26 1.51(3) . ?

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
O3 Zn1 O8 115.2(2) 7_556 5_556 ?
O3 Zn1 O12 109.69(18) 7_556 5_656 ?
O8 Zn1 O12 122.2(2) 5_556 5_656 ?
O3 Zn1 O1 95.18(18) 7_556 . ?
O8 Zn1 O1 99.94(18) 5_556 . ?
O12 Zn1 O1 110.48(17) 5_656 . ?
O5 Zn2 O2 123.86(19) . . ?
O5 Zn2 O10 117.45(18) . 6 ?
O2 Zn2 O10 106.22(18) . 6 ?
O5 Zn2 O11 103.77(19) . 5_656 ?
O2 Zn2 O11 106.47(19) . 5_656 ?
O10 Zn2 O11 94.19(17) 6 5_656 ?
O9 Zn3 O9 106.8(4) 6 5_556 ?
O9' Zn3 O9' 177.7(11) 6 5_556 ?
O9 Zn3 O13 126.62(19) 6 . ?
O9 Zn3 O13 126.62(19) 5_556 . ?
O9 Zn3 O6 88.08(19) 6 2 ?
O9 Zn3 O6 95.4(2) 5_556 2 ?
O9' Zn3 O6 89.5(5) 6 2 ?
O9' Zn3 O6 90.6(5) 5_556 2 ?
O13 Zn3 O6 87.07(13) . 2 ?
O9 Zn3 O6 95.4(2) 6 . ?
O9 Zn3 O6 88.08(19) 5_556 . ?
O9' Zn3 O6 90.6(5) 6 . ?
O9' Zn3 O6 89.5(5) 5_556 . ?
O13 Zn3 O6 87.07(13) . . ?
O6 Zn3 O6 174.1(3) 2 . ?
O9' Zn3 O13' 123.1(8) 6 . ?
O9' Zn3 O13' 59.2(8) 5_556 . ?
O6 Zn3 O13' 86.5(6) 2 . ?
O6 Zn3 O13' 88.5(6) . . ?
O9' Zn3 O13' 59.2(8) 6 2 ?
O9' Zn3 O13' 123.1(8) 5_556 2 ?
O6 Zn3 O13' 88.5(6) 2 2 ?
O6 Zn3 O13' 86.5(6) . 2 ?
O13' Zn3 O13' 63.9(11) . 2 ?
C1 O1 Zn1 135.9(4) . . ?
C1 O2 Zn2 130.5(3) . . ?
C8 O3 Zn1 127.0(4) . 7_556 ?
C9 O5 Zn2 116.7(3) . . ?
C9 O6 Zn3 142.5(4) . . ?
C22 O8 Zn1 126.0(4) . 5_556 ?
C23 O9 Zn3 140.6(6) . 5_556 ?
C23 O9' Zn3 126.4(13) . 5_556 ?
C23 O10 Zn2 120.3(4) . 6_556 ?
C24 O11 Zn2 147.4(4) . 5_656 ?
C24 O12 Zn1 122.9(3) . 5_656 ?
O1 C1 O2 125.9(5) . . ?
O1 C1 C2 117.9(5) . . ?
O2 C1 C2 116.3(4) . . ?
C3 C2 C7 119.6(5) . . ?
C3 C2 C1 119.4(4) . . ?
C7 C2 C1 120.9(5) . . ?
C2 C3 C4 120.3(4) . . ?
C3 C4 C5 119.3(5) . . ?
C3 C4 C8 120.3(5) . . ?
C5 C4 C8 120.3(5) . . ?
C4 C5 C6 121.1(5) . . ?
C7 C6 C5 118.5(5) . . ?
C7 C6 C6 120.6(3) . 2 ?
C5 C6 C6 120.9(3) . 2 ?
C6 C7 C2 121.2(5) . . ?
O4 C8 O3 124.8(6) . . ?
O4 C8 C4 119.8(5) . . ?
O3 C8 C4 115.4(5) . . ?
O6 C9 O5 123.0(5) . . ?
O6 C9 C10 120.6(5) . . ?
O5 C9 C10 116.2(5) . . ?
C11 C10 C15 119.3(5) . . ?
C11 C10 C9 120.5(5) . . ?
C15 C10 C9 120.0(5) . . ?
C10 C11 C12 120.3(5) . . ?
C13 C12 C11 119.8(5) . . ?
C13 C12 C22 118.7(5) . . ?
C11 C12 C22 121.4(5) . . ?
C12 C13 C14 120.4(5) . . ?
C15 C14 C13 118.7(4) . . ?
C15 C14 C16 120.9(5) . . ?
C13 C14 C16 120.3(4) . . ?
C14 C15 C10 121.4(5) . . ?
C17 C16 C21 119.5(5) . . ?
C17 C16 C14 119.2(5) . . ?
C21 C16 C14 121.2(4) . . ?
C16 C17 C18 120.3(5) . . ?
C17 C18 C19 119.8(5) . . ?
C17 C18 C23 119.1(5) . . ?
C19 C18 C23 120.9(5) . . ?
C20 C19 C18 119.6(5) . . ?
C21 C20 C19 120.3(5) . . ?
C21 C20 C24 120.7(4) . . ?
C19 C20 C24 119.0(4) . . ?
C20 C21 C16 120.3(5) . . ?
O7 C22 O8 124.8(6) . . ?
O7 C22 C12 120.4(5) . . ?
O8 C22 C12 114.8(5) . . ?
O10 C23 O9 124.3(6) . . ?
O10 C23 O9' 112.2(10) . . ?
O10 C23 C18 116.5(5) . . ?
O9 C23 C18 118.1(6) . . ?
O9' C23 C18 110.9(9) . . ?
O11 C24 O12 125.1(5) . . ?
O11 C24 C20 116.9(5) . . ?
O12 C24 C20 118.0(4) . . ?
C25 N1 C26 104.9(14) . . ?

_refine_diff_density_max         1.229
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.197

_shelxl_version_number           2013-2

