 
data_4 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
  'C56 H80 Cl16 N16 O16 Zn4'  
_chemical_formula_weight         2062.04 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 'H'  'H'   0.0000   0.0000 
 '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            monoclinic  
_symmetry_space_group_name_H-M    P2/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 
_cell_length_a                    7.1661(3) 
_cell_length_b                    15.0840(6) 
_cell_length_c                    19.1836(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  103.732(4) 
_cell_angle_gamma                 90.00 
_cell_volume                      2014.35(15) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     103(2) 
_cell_measurement_reflns_used     6468  
_cell_measurement_theta_min       2.6030
_cell_measurement_theta_max       30.4290
 
_exptl_crystal_description        cuboid  
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.700 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1048 
_exptl_absorpt_coefficient_mu     1.778 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.75105 
_exptl_absorpt_correction_T_max  1.00000 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       103(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    'XtaLAB Synergy R, DW system, HyPix'  
_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             14558 
_diffrn_reflns_av_R_equivalents   0.0294 
_diffrn_reflns_av_sigmaI/netI     0.0342 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          2.57 
_diffrn_reflns_theta_max          30.98 
_reflns_number_total              6299 
_reflns_number_gt                 4184 
_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)+(0.0100P)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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5027 
_refine_ls_number_parameters      220 
_refine_ls_number_restraints      9 
_refine_ls_R_factor_all           0.1148 
_refine_ls_R_factor_gt            0.1021 
_refine_ls_wR_factor_ref          0.2102 
_refine_ls_wR_factor_gt           0.2082 
_refine_ls_goodness_of_fit_ref    1.052 
_refine_ls_restrained_S_all       1.136 
_refine_ls_shift/su_max           0.004 
_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 
N1 N -0.9735(3) 0.01912(15) -0.62016(10) 0.0127(6) Uani 1 1 d D . . 
H1A H -0.9322 -0.0367 -0.6066 0.019 Uiso 1 1 d RD . . 
H1B H -0.9469 0.0321 -0.6631 0.019 Uiso 1 1 d RD . . 
H1C H -1.1025 0.0226 -0.6244 0.019 Uiso 1 1 d RD . . 
O1 O -0.6425(5) 0.3552(2) -0.42879(17) 0.0134(3) Uani 0.50 1 d P A 1 
C7 C -0.6026(7) 0.2759(4) -0.4125(3) 0.0134(3) Uani 0.50 1 d P A 1 
N2 N -0.4814(6) 0.2532(3) -0.3497(2) 0.0134(3) Uani 0.50 1 d P A 1 
O1' O -0.6396(5) 0.3550(3) -0.42943(19) 0.0134(3) Uani 0.50 1 d P A 2 
C7' C -0.6026(8) 0.2759(4) -0.4124(3) 0.0134(3) Uani 0.50 1 d P A 2 
N2' N -0.4808(7) 0.2526(3) -0.3496(2) 0.0134(3) Uani 0.50 1 d P A 2 
C1 C -0.8728(4) 0.08288(18) -0.56520(13) 0.0134(3) Uani 1 1 d . A . 
C2 C -0.7410(4) 0.05349(18) -0.50516(12) 0.0134(3) Uani 1 1 d . . . 
H2A H -0.7124 -0.0079 -0.4987 0.016 Uiso 1 1 calc R . . 
C3 C -0.6511(4) 0.11444(19) -0.45456(13) 0.0159(7) Uani 1 1 d . A . 
H3C H -0.5606 0.0950 -0.4128 0.019 Uiso 1 1 calc R . . 
C4 C -0.6930(3) 0.20503(17) -0.46469(12) 0.0099(7) Uani 1 1 d . . . 
C5 C -0.8269(3) 0.23361(18) -0.52585(12) 0.0098(6) Uani 1 1 d . A . 
H5C H -0.8549 0.2950 -0.5329 0.012 Uiso 1 1 calc R . . 
C6 C -0.9193(4) 0.17203(18) -0.57657(12) 0.0117(7) Uani 1 1 d . . . 
H6A H -1.0121 0.1906 -0.6180 0.014 Uiso 1 1 calc R A . 
O2 O -1.1448(3) 0.14545(13) -0.42696(9) 0.0193(6) Uani 1 1 d . . . 
N3 N -0.9866(3) 0.24699(16) -0.34968(10) 0.0178(7) Uani 1 1 d D . . 
H3A H -0.9388 0.2018 -0.3203 0.021 Uiso 1 1 d RD . . 
H3B H -0.9212 0.2961 -0.3561 0.021 Uiso 1 1 d RD . . 
N4 N -1.4619(3) 0.48043(15) -0.61903(10) 0.0131(6) Uani 1 1 d D . . 
H4A H -1.4013 0.4816 -0.6557 0.016 Uiso 1 1 calc R . . 
H4B H -1.4573 0.5353 -0.5990 0.016 Uiso 1 1 calc RD . . 
H4C H -1.5866 0.4641 -0.6362 0.016 Uiso 1 1 calc R . . 
C8 C -1.1919(4) 0.29570(18) -0.46272(13) 0.0134(3) Uani 1 1 d . . . 
C9 C -1.1536(3) 0.38554(18) -0.45173(12) 0.0111(7) Uani 1 1 d . . . 
H9A H -1.0660 0.4048 -0.4091 0.013 Uiso 1 1 calc R . . 
C10 C -1.2425(3) 0.44768(18) -0.50270(12) 0.0119(7) Uani 1 1 d . . . 
H10A H -1.2187 0.5093 -0.4949 0.014 Uiso 1 1 calc R . . 
C11 C -1.3674(3) 0.41741(17) -0.56545(12) 0.0100(6) Uani 1 1 d . . . 
C12 C -1.4026(3) 0.32890(18) -0.57764(13) 0.0125(7) Uani 1 1 d . . . 
H12A H -1.4869 0.3099 -0.6211 0.015 Uiso 1 1 calc R . . 
C13 C -1.3163(4) 0.26697(18) -0.52714(12) 0.0139(7) Uani 1 1 d . . . 
H13A H -1.3406 0.2055 -0.5358 0.017 Uiso 1 1 calc R . . 
C14 C -1.1040(4) 0.22391(18) -0.41132(12) 0.0119(7) Uani 1 1 d . . . 
Zn2 Zn -0.5000 -0.00322(3) -0.2500 0.01102(12) Uani 1 2 d S . . 
Cl3 Cl -0.74978(9) 0.08415(5) -0.24172(3) 0.01678(17) Uani 1 1 d . . . 
Cl8 Cl -0.42537(9) -0.09157(5) -0.15132(3) 0.01676(18) Uani 1 1 d . . . 
Zn1 Zn -1.0000 0.50894(3) -0.2500 0.01045(11) Uani 1 2 d S . . 
Cl4 Cl -0.75210(9) 0.42044(4) -0.26084(3) 0.01489(17) Uani 1 1 d . . . 
Cl7 Cl -1.09491(10) 0.59309(5) -0.34946(3) 0.0215(2) Uani 1 1 d . . . 
O5 O -0.5000 0.6256(3) -0.2500 0.1068(13) Uani 1 2 d S . . 
H5D H -0.4356 0.6077 -0.2094 0.128 Uiso 1 1 d R . . 
O6 O 0.0000 -0.12503(5) -0.2500 0.1068(13) Uani 0.50 2 d SPD B 1 
O6' O 0.0000 -0.11607(6) -0.2500 0.1068(13) Uani 0.50 2 d SPD C 2 
H6WA H -0.0852 -0.0931 -0.2572 0.160 Uiso 1 1 d RD C 2 
O7' O -1.2309(8) 0.76452(12) -0.27426(7) 0.1068(13) Uani 0.50 1 d PD D 1 
O7 O -1.2281(8) 0.75361(14) -0.26092(8) 0.1068(13) Uani 0.50 1 d PD E 2 
H7A H -1.3150 0.7140 -0.2672 0.160 Uiso 1 1 d R E 2 
H7B H -1.2351 0.7857 -0.2252 0.160 Uiso 1 1 d R E 2 
 
 
_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 
N1 C1 1.482(3) . ? 
N1 H1A 0.9100 . ? 
N1 H1B 0.9100 . ? 
N1 H1C 0.9100 . ? 
O1 C7 1.253(7) . ? 
C7 N2 1.350(6) . ? 
C7 C4 1.502(6) . ? 
O1' C7' 1.249(7) . ? 
C7' N2' 1.356(6) . ? 
C7' C4 1.503(6) . ? 
C1 C2 1.378(3) . ? 
C1 C6 1.390(4) . ? 
C2 C3 1.380(3) . ? 
C2 H2A 0.9500 . ? 
C3 C4 1.403(4) . ? 
C3 H3C 0.9500 . ? 
C4 C5 1.396(3) . ? 
C5 C6 1.394(3) . ? 
C5 H5C 0.9500 . ? 
C6 H6A 0.9500 . ? 
O2 C14 1.239(3) . ? 
N3 C14 1.325(3) . ? 
N3 H3A 0.8998 . ? 
N3 H3B 0.9000 . ? 
N4 C11 1.445(3) . ? 
N4 H4A 0.9100 . ? 
N4 H4B 0.9100 . ? 
N4 H4C 0.9100 . ? 
C8 C9 1.389(4) . ? 
C8 C13 1.410(3) . ? 
C8 C14 1.499(3) . ? 
C9 C10 1.395(3) . ? 
C9 H9A 0.9500 . ? 
C10 C11 1.395(3) . ? 
C10 H10A 0.9500 . ? 
C11 C12 1.368(4) . ? 
C12 C13 1.382(3) . ? 
C12 H12A 0.9500 . ? 
C13 H13A 0.9500 . ? 
Zn2 Cl3 2.2585(7) 2_454 ? 
Zn2 Cl3 2.2585(7) . ? 
Zn2 Cl8 2.2726(7) . ? 
Zn2 Cl8 2.2726(7) 2_454 ? 
Zn1 Cl7 2.2579(7) 2_354 ? 
Zn1 Cl7 2.2579(7) . ? 
Zn1 Cl4 2.2708(7) 2_354 ? 
Zn1 Cl4 2.2708(7) . ? 
O5 H5D 0.8500 . ? 
O6 H6WA 0.7640 . ? 
O6' H6WA 0.6870 . ? 
O7' H7A 0.9996 . ? 
O7' H7B 1.0008 . ? 
O7 H7A 0.8499 . ? 
O7 H7B 0.8499 . ? 
 
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 
C1 N1 H1A 109.1 . . ? 
C1 N1 H1B 109.5 . . ? 
H1A N1 H1B 109.5 . . ? 
C1 N1 H1C 109.8 . . ? 
H1A N1 H1C 109.5 . . ? 
H1B N1 H1C 109.5 . . ? 
O1 C7 N2 121.6(5) . . ? 
O1 C7 C4 118.4(4) . . ? 
N2 C7 C4 119.9(4) . . ? 
O1' C7' N2' 122.1(5) . . ? 
O1' C7' C4 118.3(4) . . ? 
N2' C7' C4 119.6(5) . . ? 
C2 C1 C6 122.2(2) . . ? 
C2 C1 N1 120.5(2) . . ? 
C6 C1 N1 117.3(2) . . ? 
C1 C2 C3 119.1(3) . . ? 
C1 C2 H2A 120.4 . . ? 
C3 C2 H2A 120.4 . . ? 
C2 C3 C4 120.2(2) . . ? 
C2 C3 H3C 119.9 . . ? 
C4 C3 H3C 119.9 . . ? 
C5 C4 C3 119.9(2) . . ? 
C5 C4 C7 116.3(3) . . ? 
C3 C4 C7 123.8(3) . . ? 
C5 C4 C7' 116.3(3) . . ? 
C3 C4 C7' 123.8(3) . . ? 
C7 C4 C7' 0.0(4) . . ? 
C4 C5 C6 119.9(2) . . ? 
C4 C5 H5C 120.0 . . ? 
C6 C5 H5C 120.0 . . ? 
C1 C6 C5 118.6(2) . . ? 
C1 C6 H6A 120.7 . . ? 
C5 C6 H6A 120.7 . . ? 
C14 N3 H3A 115.3 . . ? 
C14 N3 H3B 109.6 . . ? 
H3A N3 H3B 125.2 . . ? 
C11 N4 H4A 109.5 . . ? 
C11 N4 H4B 109.5 . . ? 
H4A N4 H4B 109.5 . . ? 
C11 N4 H4C 109.5 . . ? 
H4A N4 H4C 109.5 . . ? 
H4B N4 H4C 109.5 . . ? 
C9 C8 C13 119.6(2) . . ? 
C9 C8 C14 124.6(2) . . ? 
C13 C8 C14 115.7(2) . . ? 
C8 C9 C10 120.6(2) . . ? 
C8 C9 H9A 119.7 . . ? 
C10 C9 H9A 119.7 . . ? 
C11 C10 C9 118.5(2) . . ? 
C11 C10 H10A 120.7 . . ? 
C9 C10 H10A 120.7 . . ? 
C12 C11 C10 121.4(2) . . ? 
C12 C11 N4 118.9(2) . . ? 
C10 C11 N4 119.7(2) . . ? 
C11 C12 C13 120.4(2) . . ? 
C11 C12 H12A 119.8 . . ? 
C13 C12 H12A 119.8 . . ? 
C12 C13 C8 119.4(2) . . ? 
C12 C13 H13A 120.3 . . ? 
C8 C13 H13A 120.3 . . ? 
O2 C14 N3 122.1(2) . . ? 
O2 C14 C8 119.5(2) . . ? 
N3 C14 C8 118.4(2) . . ? 
Cl3 Zn2 Cl3 108.60(4) 2_454 . ? 
Cl3 Zn2 Cl8 111.53(2) 2_454 . ? 
Cl3 Zn2 Cl8 108.50(2) . . ? 
Cl3 Zn2 Cl8 108.50(2) 2_454 2_454 ? 
Cl3 Zn2 Cl8 111.53(2) . 2_454 ? 
Cl8 Zn2 Cl8 108.20(4) . 2_454 ? 
Cl7 Zn1 Cl7 111.59(4) 2_354 . ? 
Cl7 Zn1 Cl4 109.78(2) 2_354 2_354 ? 
Cl7 Zn1 Cl4 108.82(2) . 2_354 ? 
Cl7 Zn1 Cl4 108.82(2) 2_354 . ? 
Cl7 Zn1 Cl4 109.78(2) . . ? 
Cl4 Zn1 Cl4 107.99(4) 2_354 . ? 
H7A O7' H7B 87.9 . . ? 
H7A O7 H7B 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 
C6 C1 C2 C3 -0.3(4) . . . . ? 
N1 C1 C2 C3 -179.3(2) . . . . ? 
C1 C2 C3 C4 -0.4(4) . . . . ? 
C2 C3 C4 C5 0.4(4) . . . . ? 
C2 C3 C4 C7 179.8(3) . . . . ? 
C2 C3 C4 C7' 179.8(4) . . . . ? 
O1 C7 C4 C5 -4.5(6) . . . . ? 
N2 C7 C4 C5 175.6(4) . . . . ? 
O1 C7 C4 C3 176.1(4) . . . . ? 
N2 C7 C4 C3 -3.9(7) . . . . ? 
O1 C7 C4 C7' -148(100) . . . . ? 
N2 C7 C4 C7' 33(100) . . . . ? 
O1' C7' C4 C5 -5.9(6) . . . . ? 
N2' C7' C4 C5 175.7(4) . . . . ? 
O1' C7' C4 C3 174.7(4) . . . . ? 
N2' C7' C4 C3 -3.8(7) . . . . ? 
O1' C7' C4 C7 31(100) . . . . ? 
N2' C7' C4 C7 -147(100) . . . . ? 
C3 C4 C5 C6 0.3(4) . . . . ? 
C7 C4 C5 C6 -179.2(3) . . . . ? 
C7' C4 C5 C6 -179.1(3) . . . . ? 
C2 C1 C6 C5 1.0(4) . . . . ? 
N1 C1 C6 C5 -180.0(2) . . . . ? 
C4 C5 C6 C1 -1.0(4) . . . . ? 
C13 C8 C9 C10 2.3(4) . . . . ? 
C14 C8 C9 C10 -180.0(3) . . . . ? 
C8 C9 C10 C11 -1.3(4) . . . . ? 
C9 C10 C11 C12 -0.3(4) . . . . ? 
C9 C10 C11 N4 179.8(2) . . . . ? 
C10 C11 C12 C13 0.8(4) . . . . ? 
N4 C11 C12 C13 -179.3(2) . . . . ? 
C11 C12 C13 C8 0.2(4) . . . . ? 
C9 C8 C13 C12 -1.8(4) . . . . ? 
C14 C8 C13 C12 -179.7(2) . . . . ? 
C9 C8 C14 O2 -178.5(3) . . . . ? 
C13 C8 C14 O2 -0.7(4) . . . . ? 
C9 C8 C14 N3 2.6(4) . . . . ? 
C13 C8 C14 N3 -179.6(2) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
N1 H1A O2  0.91 1.80 2.708(3) 175.4 3_354 
N4 H4A O5  0.91 2.40 2.936(3) 117.3 3_364 
O5 H5D N4  0.85 2.23 2.936(3) 140.8 4_666 
O7 H7A O5  0.85 1.96 2.786(5) 162.6 1_455 
N1 H1B O6'  0.91 2.06 2.856(2) 145.9 3_454 
N1 H1B O6  0.91 2.14 2.927(2) 144.0 3_454 
N4 H4B O1'  0.91 1.83 2.690(5) 157.3 3_364 
N4 H4B O1  0.91 1.83 2.687(4) 156.5 3_364  

_diffrn_measured_fraction_theta_max    0.981 
_diffrn_reflns_theta_full              30.98 
_diffrn_measured_fraction_theta_full   0.981 
_refine_diff_density_max    2.450 
_refine_diff_density_min   -2.010 
_refine_diff_density_rms    0.179 
