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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
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#  as required by the journal to which it was submitted.
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data_KT0211

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H46 N3 O17 Zn3, 3(C3 H7 N O)'
_chemical_formula_sum            'C63 H67 N6 O20 Zn3'
_chemical_formula_weight         1424.33

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      orthorhombic
_space_group_IT_number           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'

_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+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'

_cell_length_a                   26.846(5)
_cell_length_b                   27.178(5)
_cell_length_c                   9.766(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7125(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14632
_cell_measurement_theta_min      1.07
_cell_measurement_theta_max      30.92

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_F_000             2948
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.073
_shelx_estimated_absorpt_T_min   0.938
_shelx_estimated_absorpt_T_max   0.958
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Australian Synchrotron'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            146327
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_av_R_equivalents  0.0982
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.066
_diffrn_reflns_theta_max         30.923
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             11559
_reflns_number_gt                5224
_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_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

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 -0.250 0.250 0.331 992 195 ' '
2 0.250 0.750 0.658 992 196 ' '
3 0.250 0.250 0.768 226 41 ' '
4 0.750 0.750 0.232 226 42 ' '
_platon_squeeze_details          
;
 Squeeze results suggest approx 3 DMF per formula unit.
 These solvent molecules are included in the refined formula.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.2000P)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         11559
_refine_ls_number_parameters     379
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.2225
_refine_ls_R_factor_gt           0.1213
_refine_ls_wR_factor_ref         0.3981
_refine_ls_wR_factor_gt          0.3507
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_restrained_S_all      1.203
_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 0.90436(4) 0.2500 0.05862(10) 0.0956(4) Uani 1 2 d S T P . .
Zn2 Zn 0.99961(3) 0.2500 -0.18608(8) 0.0797(4) Uani 1 2 d S T P . .
Zn3 Zn 0.7500 0.51170(6) 0.09632(13) 0.1102(5) Uani 1 2 d S T P . .
O1 O 1.0422(3) 0.2500 -0.0228(6) 0.110(2) Uani 1 2 d S T P . .
O2 O 0.9786(3) 0.2500 0.1177(7) 0.1039(18) Uani 1 2 d S T P . .
O3 O 1.0060(6) 0.2500 0.6110(9) 0.185(5) Uani 1 2 d S T P . .
O4 O 1.0747(7) 0.2500 0.6902(10) 0.210(6) Uani 1 2 d S T P . .
O5 O 0.9614(3) 0.31057(17) -0.1842(5) 0.136(2) Uani 1 1 d . . . . .
O6 O 0.9010(2) 0.3109(2) -0.0301(7) 0.139(2) Uani 1 1 d . . . . .
O7A O 0.8064(5) 0.5142(5) -0.0929(14) 0.145(5) Uani 0.663(19) 1 d D . P A 2
O7B O 0.8320(6) 0.5389(4) -0.1379(16) 0.095(6) Uani 0.337(19) 1 d D . P A 1
O8A O 0.8053(3) 0.4597(7) 0.0370(14) 0.139(6) Uani 0.663(19) 1 d D . P A 2
O8B O 0.8078(6) 0.4814(6) -0.0207(16) 0.067(4) Uani 0.337(19) 1 d D . P A 1
O9 O 0.8803(5) 0.2500 0.2420(10) 0.238(8) Uani 1 2 d S T P . .
O10 O 0.8259(5) 0.2500 0.007(2) 0.289(10) Uani 1 2 d S T P . .
O12 O 0.8017(4) 0.5608(4) 0.1997(12) 0.240(5) Uani 1 1 d D . . . .
O13 O 0.7500 0.4687(7) 0.2614(11) 0.273(10) Uani 1 2 d DS T P A .
N1 N 0.8648(4) 0.6149(5) 0.2196(14) 0.257(7) Uiso 1 1 d D . . . .
N2 N 0.7500 0.4526(5) 0.4874(11) 0.176(5) Uiso 1 2 d DS . P . .
C1 C 1.0583(3) 0.2500 0.2088(6) 0.0771(19) Uani 1 2 d S T P . .
C2 C 1.0408(4) 0.2500 0.3462(8) 0.092(3) Uani 1 2 d S T P . .
H2 H 1.0059 0.2500 0.3625 0.111 Uiso 1 2 calc R U P . .
C3 C 1.0721(4) 0.2500 0.4538(7) 0.092(3) Uani 1 2 d S T P . .
C4 C 1.1208(4) 0.2500 0.4311(8) 0.101(3) Uani 1 2 d S T P . .
H4 H 1.1424 0.2500 0.5081 0.121 Uiso 1 2 calc R U P . .
C5 C 1.1427(4) 0.2500 0.2968(9) 0.093(2) Uani 1 2 d S T P . .
C6 C 1.1099(3) 0.2500 0.1905(7) 0.082(2) Uani 1 2 d S T P . .
H6 H 1.1227 0.2500 0.0998 0.099 Uiso 1 2 calc R U P . .
C7 C 1.0233(4) 0.2500 0.0947(8) 0.088(2) Uani 1 2 d S T P . .
C8 C 1.0500(7) 0.2500 0.5962(11) 0.122(4) Uani 1 2 d S T P . .
C9 C 1.1968(4) 0.2500 0.2829(8) 0.089(2) Uani 1 2 d S T P . .
C10 C 1.2232(3) 0.2949(3) 0.2822(10) 0.128(3) Uani 1 1 d . . . . .
C11 C 1.1975(4) 0.3392(4) 0.2787(17) 0.212(7) Uani 1 1 d . . . . .
H11 H 1.1622 0.3401 0.2825 0.254 Uiso 1 1 calc R U . . .
C12 C 1.2247(6) 0.3813(5) 0.270(3) 0.343(16) Uani 1 1 d . . . . .
H12 H 1.2077 0.4119 0.2631 0.411 Uiso 1 1 calc R U . . .
C13 C 0.9154(2) 0.3831(2) -0.1646(6) 0.0852(15) Uani 1 1 d . . . . .
C14 C 0.8772(2) 0.4085(2) -0.1015(6) 0.0839(15) Uani 1 1 d . . . . .
H14 H 0.8582 0.3929 -0.0320 0.101 Uiso 1 1 calc R U . . .
C15 C 0.8671(2) 0.4543(3) -0.1370(8) 0.100(2) Uani 1 1 d D . . . .
C16 C 0.8975(3) 0.4782(2) -0.2437(9) 0.109(3) Uani 1 1 d . . . . .
H16 H 0.8905 0.5111 -0.2706 0.130 Uiso 1 1 calc R U . . .
C17 C 0.9353(2) 0.4533(2) -0.3034(6) 0.0875(17) Uani 1 1 d . . . . .
C18 C 0.9440(2) 0.4055(2) -0.2630(6) 0.0778(13) Uani 1 1 d . . . . .
H18 H 0.9704 0.3876 -0.3043 0.093 Uiso 1 1 calc R U . . .
C19 C 0.9283(3) 0.3312(3) -0.1240(6) 0.0925(16) Uani 1 1 d . . . . .
C20A C 0.8242(6) 0.4767(6) -0.0601(17) 0.142(12) Uani 0.663(19) 1 d D . P A 2
C20B C 0.8353(8) 0.4980(4) -0.102(3) 0.091(9) Uani 0.337(19) 1 d D . P A 1
C21 C 0.9675(2) 0.4763(2) -0.4053(7) 0.0875(16) Uani 1 1 d . . . . .
C22 C 1.0155(3) 0.4927(2) -0.3657(8) 0.100(2) Uani 1 1 d . . . . .
C23 C 1.0327(3) 0.4857(3) -0.2257(8) 0.115(2) Uani 1 1 d . . . . .
H23 H 1.0114 0.4709 -0.1599 0.138 Uiso 1 1 calc R U . . .
C24 C 1.0794(3) 0.5004(3) -0.1891(9) 0.119(3) Uani 1 1 d . . . . .
H24 H 1.0911 0.4948 -0.0987 0.143 Uiso 1 1 calc R U . . .
C25 C 0.9524(2) 0.4855(2) -0.5400(8) 0.0957(19) Uani 1 1 d . . . . .
C26 C 0.9046(3) 0.4683(3) -0.5884(8) 0.114(2) Uani 1 1 d . . . . .
H26 H 0.8831 0.4509 -0.5282 0.136 Uiso 1 1 calc R U . . .
C27 C 0.8906(3) 0.4767(4) -0.7174(10) 0.134(3) Uani 1 1 d . . . . .
H27 H 0.8583 0.4663 -0.7455 0.161 Uiso 1 1 calc R U . . .
C28 C 0.8278(5) 0.5898(5) 0.1368(9) 0.218(6) Uiso 1 1 d D . . . .
H28 H 0.8241 0.5956 0.0414 0.262 Uiso 1 1 calc R U . . .
C29 C 0.8733(10) 0.6029(9) 0.3555(15) 0.304(10) Uiso 1 1 d D . . . .
H29A H 0.8459 0.5826 0.3895 0.455 Uiso 0.5 1 calc R U P . .
H29B H 0.8755 0.6332 0.4099 0.455 Uiso 0.5 1 calc R U P . .
H29C H 0.9047 0.5847 0.3630 0.455 Uiso 0.5 1 calc R U P . .
H29D H 0.9048 0.6177 0.3855 0.455 Uiso 0.5 1 calc R U P . .
H29E H 0.8752 0.5671 0.3651 0.455 Uiso 0.5 1 calc R U P . .
H29F H 0.8460 0.6156 0.4120 0.455 Uiso 0.5 1 calc R U P . .
C30 C 0.8996(7) 0.6417(8) 0.1461(18) 0.293(10) Uiso 1 1 d D . . . .
H30A H 0.8876 0.6466 0.0523 0.439 Uiso 0.5 1 calc R U P . .
H30B H 0.9312 0.6236 0.1440 0.439 Uiso 0.5 1 calc R U P . .
H30C H 0.9047 0.6737 0.1900 0.439 Uiso 0.5 1 calc R U P . .
H30D H 0.9281 0.6494 0.2052 0.439 Uiso 0.5 1 calc R U P . .
H30E H 0.8845 0.6723 0.1135 0.439 Uiso 0.5 1 calc R U P . .
H30F H 0.9110 0.6222 0.0676 0.439 Uiso 0.5 1 calc R U P . .
C31 C 0.7500 0.4874(4) 0.3750(14) 0.211(10) Uiso 1 2 d DS . P A .
H31 H 0.7500 0.5220 0.3886 0.254 Uiso 1 2 calc R U P . .
C32 C 0.7500 0.4773(8) 0.6114(18) 0.277(14) Uiso 1 2 d DS . P B .
H32A H 0.7500 0.4535 0.6866 0.415 Uiso 0.5 2 calc R U P . .
H32B H 0.7202 0.4980 0.6177 0.415 Uiso 0.25 1 calc R U P . .
H32C H 0.7798 0.4980 0.6177 0.415 Uiso 0.25 1 calc R U P . .
H32D H 0.7500 0.5129 0.5947 0.415 Uiso 0.5 2 calc R U P . .
H32E H 0.7798 0.4683 0.6636 0.415 Uiso 0.25 1 calc R U P . .
H32F H 0.7202 0.4683 0.6636 0.415 Uiso 0.25 1 calc R U P . .
C33 C 0.7789(9) 0.4109(7) 0.469(3) 0.215(12) Uiso 0.5 1 d D . P B -1
H33A H 0.7755 0.3994 0.3740 0.323 Uiso 0.25 1 calc R U P B -1
H33B H 0.7678 0.3850 0.5314 0.323 Uiso 0.25 1 calc R U P B -1
H33C H 0.8139 0.4188 0.4873 0.323 Uiso 0.25 1 calc R U P B -1
H33D H 0.7959 0.4027 0.5545 0.323 Uiso 0.25 1 calc R U P B -1
H33E H 0.8037 0.4171 0.3970 0.323 Uiso 0.25 1 calc R U P B -1
H33F H 0.7576 0.3833 0.4412 0.323 Uiso 0.25 1 calc R U P B -1


_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 O6 1.870(6) 8_565 ?
Zn1 O6 1.870(6) . ?
Zn1 O9 1.903(8) . ?
Zn1 O2 2.075(7) . ?
Zn1 O10 2.167(15) . ?
Zn2 O5 1.939(5) 8_565 ?
Zn2 O5 1.939(5) . ?
Zn2 O1 1.962(7) . ?
Zn2 O3 1.989(8) 1_554 ?
Zn2 O4 2.349(14) 1_554 ?
Zn2 C8 2.520(11) 1_554 ?
Zn3 O13 1.992(12) . ?
Zn3 O8B 2.095(17) . ?
Zn3 O8B 2.095(17) 7_755 ?
Zn3 O8A 2.128(13) . ?
Zn3 O8A 2.128(13) 7_755 ?
Zn3 O12 2.175(9) . ?
Zn3 O12 2.175(9) 7_755 ?
Zn3 O7A 2.391(13) 7_755 ?
Zn3 O7A 2.391(13) . ?
O1 C7 1.254(9) . ?
O2 C7 1.220(11) . ?
O3 C8 1.191(18) . ?
O3 Zn2 1.989(8) 1_556 ?
O4 C8 1.13(2) . ?
O4 Zn2 2.349(14) 1_556 ?
O5 C19 1.205(8) . ?
O6 C19 1.297(8) . ?
O7A C20A 1.171(8) . ?
O7B C20B 1.172(8) . ?
O8A C20A 1.171(8) . ?
O8B C20B 1.171(8) . ?
O12 C28 1.2199(10) . ?
O13 C31 1.2199(10) . ?
N1 C29 1.386(8) . ?
N1 C30 1.386(8) . ?
N1 C28 1.4499(10) . ?
N2 C32 1.385(8) . ?
N2 C33 1.386(8) . ?
N2 C31 1.4498(10) . ?
C1 C6 1.396(12) . ?
C1 C2 1.421(9) . ?
C1 C7 1.458(13) . ?
C2 C3 1.346(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.326(16) . ?
C3 C8 1.512(12) . ?
C4 C5 1.437(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.361(13) . ?
C5 C9 1.459(14) . ?
C6 H6 0.9500 . ?
C8 Zn2 2.520(11) 1_556 ?
C9 C10 1.412(10) . ?
C9 C10 1.412(10) 8_565 ?
C10 C11 1.389(13) . ?
C10 C10 1.437(16) 7_855 ?
C11 C12 1.360(17) . ?
C11 H11 0.9500 . ?
C12 C12 1.36(3) 7_855 ?
C12 H12 0.9500 . ?
C13 C18 1.372(9) . ?
C13 C14 1.381(9) . ?
C13 C19 1.506(9) . ?
C14 C15 1.321(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.475(12) . ?
C15 C20B 1.501(5) . ?
C15 C20A 1.502(5) . ?
C16 C17 1.352(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(8) . ?
C17 C21 1.460(9) . ?
C18 H18 0.9500 . ?
C21 C25 1.399(9) . ?
C21 C22 1.415(8) . ?
C22 C25 1.394(11) 5_764 ?
C22 C23 1.455(9) . ?
C23 C24 1.364(10) . ?
C23 H23 0.9500 . ?
C24 C27 1.367(13) 5_764 ?
C24 H24 0.9500 . ?
C25 C22 1.394(11) 5_764 ?
C25 C26 1.445(8) . ?
C26 C27 1.335(11) . ?
C26 H26 0.9500 . ?
C27 C24 1.368(13) 5_764 ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C29 H29D 0.9800 . ?
C29 H29E 0.9800 . ?
C29 H29F 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C30 H30D 0.9800 . ?
C30 H30E 0.9800 . ?
C30 H30F 0.9800 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C32 H32D 0.9800 . ?
C32 H32E 0.9800 . ?
C32 H32F 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 H33D 0.9800 . ?
C33 H33E 0.9800 . ?
C33 H33F 0.9800 . ?

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
O6 Zn1 O6 124.5(5) 8_565 . ?
O6 Zn1 O9 114.8(2) 8_565 . ?
O6 Zn1 O9 114.8(2) . . ?
O6 Zn1 O2 100.1(2) 8_565 . ?
O6 Zn1 O2 100.1(2) . . ?
O9 Zn1 O2 93.7(4) . . ?
O6 Zn1 O10 81.1(3) 8_565 . ?
O6 Zn1 O10 81.1(3) . . ?
O9 Zn1 O10 83.6(7) . . ?
O2 Zn1 O10 177.3(6) . . ?
O5 Zn2 O5 116.2(4) 8_565 . ?
O5 Zn2 O1 107.5(2) 8_565 . ?
O5 Zn2 O1 107.5(2) . . ?
O5 Zn2 O3 93.1(3) 8_565 1_554 ?
O5 Zn2 O3 93.1(3) . 1_554 ?
O1 Zn2 O3 139.4(5) . 1_554 ?
O5 Zn2 O4 117.3(2) 8_565 1_554 ?
O5 Zn2 O4 117.3(2) . 1_554 ?
O1 Zn2 O4 85.3(4) . 1_554 ?
O3 Zn2 O4 54.1(5) 1_554 1_554 ?
O5 Zn2 C8 107.0(2) 8_565 1_554 ?
O5 Zn2 C8 107.0(2) . 1_554 ?
O1 Zn2 C8 111.9(5) . 1_554 ?
O3 Zn2 C8 27.5(5) 1_554 1_554 ?
O4 Zn2 C8 26.6(5) 1_554 1_554 ?
O13 Zn3 O8B 102.2(5) . . ?
O13 Zn3 O8B 102.2(5) . 7_755 ?
O8B Zn3 O8B 95.5(9) . 7_755 ?
O13 Zn3 O8A 80.3(6) . . ?
O13 Zn3 O8A 80.3(6) . 7_755 ?
O8A Zn3 O8A 88.4(7) . 7_755 ?
O13 Zn3 O12 89.1(5) . . ?
O8B Zn3 O12 91.3(5) . . ?
O8B Zn3 O12 165.3(5) 7_755 . ?
O8A Zn3 O12 95.1(4) . . ?
O8A Zn3 O12 168.1(5) 7_755 . ?
O13 Zn3 O12 89.1(5) . 7_755 ?
O8B Zn3 O12 165.3(5) . 7_755 ?
O8B Zn3 O12 91.3(5) 7_755 7_755 ?
O8A Zn3 O12 168.1(5) . 7_755 ?
O8A Zn3 O12 95.1(4) 7_755 7_755 ?
O12 Zn3 O12 79.4(6) . 7_755 ?
O13 Zn3 O7A 130.0(4) . 7_755 ?
O8A Zn3 O7A 104.5(4) . 7_755 ?
O8A Zn3 O7A 50.7(5) 7_755 7_755 ?
O12 Zn3 O7A 138.3(5) . 7_755 ?
O12 Zn3 O7A 86.4(4) 7_755 7_755 ?
O13 Zn3 O7A 130.0(4) . . ?
O8A Zn3 O7A 50.7(5) . . ?
O8A Zn3 O7A 104.5(4) 7_755 . ?
O12 Zn3 O7A 86.4(4) . . ?
O12 Zn3 O7A 138.3(5) 7_755 . ?
O7A Zn3 O7A 78.6(7) 7_755 . ?
C7 O1 Zn2 120.5(7) . . ?
C7 O2 Zn1 153.3(6) . . ?
C8 O3 Zn2 101.9(10) . 1_556 ?
C8 O4 Zn2 85.2(12) . 1_556 ?
C19 O5 Zn2 142.1(5) . . ?
C19 O6 Zn1 132.5(5) . . ?
C20A O7A Zn3 91.3(8) . . ?
C20A O8A Zn3 105.2(11) . . ?
C20B O8B Zn3 133.1(11) . . ?
C28 O12 Zn3 122.0(7) . . ?
C31 O13 Zn3 119.4(10) . . ?
C29 N1 C30 120.5(12) . . ?
C29 N1 C28 122.5(12) . . ?
C30 N1 C28 114.9(12) . . ?
C32 N2 C33 120.9(12) . . ?
C32 N2 C31 110.2(14) . . ?
C33 N2 C31 115.7(12) . . ?
C6 C1 C2 116.7(8) . . ?
C6 C1 C7 122.8(6) . . ?
C2 C1 C7 120.6(8) . . ?
C3 C2 C1 122.0(9) . . ?
C3 C2 H2 119.0 . . ?
C1 C2 H2 119.0 . . ?
C4 C3 C2 119.1(7) . . ?
C4 C3 C8 122.6(11) . . ?
C2 C3 C8 118.3(11) . . ?
C3 C4 C5 123.7(9) . . ?
C3 C4 H4 118.1 . . ?
C5 C4 H4 118.1 . . ?
C6 C5 C4 115.6(9) . . ?
C6 C5 C9 124.9(7) . . ?
C4 C5 C9 119.5(9) . . ?
C5 C6 C1 122.9(6) . . ?
C5 C6 H6 118.5 . . ?
C1 C6 H6 118.5 . . ?
O2 C7 O1 124.4(9) . . ?
O2 C7 C1 119.5(6) . . ?
O1 C7 C1 116.0(8) . . ?
O4 C8 O3 118.8(12) . . ?
O4 C8 C3 121.2(16) . . ?
O3 C8 C3 120.0(14) . . ?
O4 C8 Zn2 68.2(8) . 1_556 ?
O3 C8 Zn2 50.5(6) . 1_556 ?
C3 C8 Zn2 170.6(12) . 1_556 ?
C10 C9 C10 119.6(10) . 8_565 ?
C10 C9 C5 120.1(5) . . ?
C10 C9 C5 120.1(5) 8_565 . ?
C11 C10 C9 120.0(8) . . ?
C11 C10 C10 119.8(6) . 7_855 ?
C9 C10 C10 120.2(5) . 7_855 ?
C12 C11 C10 117.7(10) . . ?
C12 C11 H11 121.2 . . ?
C10 C11 H11 121.2 . . ?
C12 C12 C11 122.5(7) 7_855 . ?
C12 C12 H12 118.8 7_855 . ?
C11 C12 H12 118.8 . . ?
C18 C13 C14 120.3(6) . . ?
C18 C13 C19 118.2(6) . . ?
C14 C13 C19 121.5(6) . . ?
C15 C14 C13 120.5(7) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 119.1(6) . . ?
C14 C15 C20B 143.3(8) . . ?
C16 C15 C20B 97.4(7) . . ?
C14 C15 C20A 114.1(9) . . ?
C16 C15 C20A 126.8(8) . . ?
C17 C16 C15 119.9(6) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 118.5(7) . . ?
C16 C17 C21 121.6(6) . . ?
C18 C17 C21 119.9(6) . . ?
C13 C18 C17 121.6(6) . . ?
C13 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
O5 C19 O6 124.5(7) . . ?
O5 C19 C13 118.5(6) . . ?
O6 C19 C13 117.0(6) . . ?
O7A C20A O8A 112.7(11) . . ?
O7A C20A C15 121.9(11) . . ?
O8A C20A C15 125.4(11) . . ?
O8B C20B O7B 121.4(12) . . ?
O8B C20B C15 102.1(11) . . ?
O7B C20B C15 136.4(11) . . ?
C25 C21 C22 117.7(6) . . ?
C25 C21 C17 123.0(5) . . ?
C22 C21 C17 119.2(6) . . ?
C25 C22 C21 121.1(6) 5_764 . ?
C25 C22 C23 118.7(6) 5_764 . ?
C21 C22 C23 120.2(7) . . ?
C24 C23 C22 120.0(8) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C27 120.0(8) . 5_764 ?
C23 C24 H24 120.0 . . ?
C27 C24 H24 120.0 5_764 . ?
C22 C25 C21 121.1(5) 5_764 . ?
C22 C25 C26 118.1(6) 5_764 . ?
C21 C25 C26 120.6(6) . . ?
C27 C26 C25 120.3(7) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C24 122.8(7) . 5_764 ?
C26 C27 H27 118.6 . . ?
C24 C27 H27 118.6 5_764 . ?
O12 C28 N1 114.60(13) . . ?
O12 C28 H28 122.7 . . ?
N1 C28 H28 122.7 . . ?
N1 C29 H29A 109.5 . . ?
N1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N1 C29 H29D 109.5 . . ?
H29A C29 H29D 141.1 . . ?
H29B C29 H29D 56.3 . . ?
H29C C29 H29D 56.3 . . ?
N1 C29 H29E 109.5 . . ?
H29A C29 H29E 56.3 . . ?
H29B C29 H29E 141.1 . . ?
H29C C29 H29E 56.3 . . ?
H29D C29 H29E 109.5 . . ?
N1 C29 H29F 109.5 . . ?
H29A C29 H29F 56.3 . . ?
H29B C29 H29F 56.3 . . ?
H29C C29 H29F 141.1 . . ?
H29D C29 H29F 109.5 . . ?
H29E C29 H29F 109.5 . . ?
N1 C30 H30A 109.5 . . ?
N1 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N1 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N1 C30 H30D 109.5 . . ?
H30A C30 H30D 141.1 . . ?
H30B C30 H30D 56.3 . . ?
H30C C30 H30D 56.3 . . ?
N1 C30 H30E 109.5 . . ?
H30A C30 H30E 56.3 . . ?
H30B C30 H30E 141.1 . . ?
H30C C30 H30E 56.3 . . ?
H30D C30 H30E 109.5 . . ?
N1 C30 H30F 109.5 . . ?
H30A C30 H30F 56.3 . . ?
H30B C30 H30F 56.3 . . ?
H30C C30 H30F 141.1 . . ?
H30D C30 H30F 109.5 . . ?
H30E C30 H30F 109.5 . . ?
O13 C31 N2 114.60(13) . . ?
O13 C31 H31 122.7 . . ?
N2 C31 H31 122.7 . . ?
N2 C32 H32A 109.5 . . ?
N2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N2 C32 H32D 109.5 . . ?
H32A C32 H32D 141.1 . . ?
H32B C32 H32D 56.3 . . ?
H32C C32 H32D 56.3 . . ?
N2 C32 H32E 109.5 . . ?
H32A C32 H32E 56.3 . . ?
H32B C32 H32E 141.1 . . ?
H32C C32 H32E 56.3 . . ?
H32D C32 H32E 109.5 . . ?
N2 C32 H32F 109.5 . . ?
H32A C32 H32F 56.3 . . ?
H32B C32 H32F 56.3 . . ?
H32C C32 H32F 141.1 . . ?
H32D C32 H32F 109.5 . . ?
H32E C32 H32F 109.5 . . ?
N2 C33 H33A 109.5 . . ?
N2 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N2 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N2 C33 H33D 109.5 . . ?
H33A C33 H33D 141.1 . . ?
H33B C33 H33D 56.3 . . ?
H33C C33 H33D 56.3 . . ?
N2 C33 H33E 109.5 . . ?
H33A C33 H33E 56.3 . . ?
H33B C33 H33E 141.1 . . ?
H33C C33 H33E 56.3 . . ?
H33D C33 H33E 109.5 . . ?
N2 C33 H33F 109.5 . . ?
H33A C33 H33F 56.3 . . ?
H33B C33 H33F 56.3 . . ?
H33C C33 H33F 141.1 . . ?
H33D C33 H33F 109.5 . . ?
H33E C33 H33F 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
O6 Zn1 O6 C19 -59.7(10) 8_565 . . . ?
O9 Zn1 O6 C19 149.0(8) . . . . ?
O2 Zn1 O6 C19 50.1(8) . . . . ?
O10 Zn1 O6 C19 -132.3(10) . . . . ?
C6 C1 C2 C3 0.000(1) . . . . ?
C7 C1 C2 C3 180.000(1) . . . . ?
C1 C2 C3 C4 0.000(1) . . . . ?
C1 C2 C3 C8 180.000(1) . . . . ?
C2 C3 C4 C5 0.000(1) . . . . ?
C8 C3 C4 C5 180.000(1) . . . . ?
C3 C4 C5 C6 0.000(1) . . . . ?
C3 C4 C5 C9 180.000(1) . . . . ?
C4 C5 C6 C1 0.000(1) . . . . ?
C9 C5 C6 C1 180.000(1) . . . . ?
C2 C1 C6 C5 0.000(1) . . . . ?
C7 C1 C6 C5 180.000(1) . . . . ?
Zn1 O2 C7 O1 0.000(1) . . . . ?
Zn1 O2 C7 C1 180.000(1) . . . . ?
Zn2 O1 C7 O2 0.000(0) . . . . ?
Zn2 O1 C7 C1 180.000(0) . . . . ?
C6 C1 C7 O2 180.000(0) . . . . ?
C2 C1 C7 O2 0.000(0) . . . . ?
C6 C1 C7 O1 0.000(1) . . . . ?
C2 C1 C7 O1 180.000(0) . . . . ?
Zn2 O4 C8 O3 0.000(2) 1_556 . . . ?
Zn2 O4 C8 C3 180.000(2) 1_556 . . . ?
Zn2 O3 C8 O4 0.000(2) 1_556 . . . ?
Zn2 O3 C8 C3 180.000(1) 1_556 . . . ?
C4 C3 C8 O4 0.000(2) . . . . ?
C2 C3 C8 O4 180.000(2) . . . . ?
C4 C3 C8 O3 180.000(1) . . . . ?
C2 C3 C8 O3 0.000(2) . . . . ?
C6 C5 C9 C10 92.8(8) . . . . ?
C4 C5 C9 C10 -87.2(8) . . . . ?
C6 C5 C9 C10 -92.8(8) . . . 8_565 ?
C4 C5 C9 C10 87.2(8) . . . 8_565 ?
C10 C9 C10 C11 178.0(9) 8_565 . . . ?
C5 C9 C10 C11 -7.4(15) . . . . ?
C10 C9 C10 C10 -0.7(12) 8_565 . . 7_855 ?
C5 C9 C10 C10 173.8(6) . . . 7_855 ?
C9 C10 C11 C12 -176.1(18) . . . . ?
C10 C10 C11 C12 3(2) 7_855 . . . ?
C10 C11 C12 C12 -3(2) . . . 7_855 ?
C18 C13 C14 C15 1.5(8) . . . . ?
C19 C13 C14 C15 178.9(5) . . . . ?
C13 C14 C15 C16 -0.9(8) . . . . ?
C13 C14 C15 C20B -174(2) . . . . ?
C13 C14 C15 C20A 179.4(10) . . . . ?
C14 C15 C16 C17 -0.2(8) . . . . ?
C20B C15 C16 C17 175.9(13) . . . . ?
C20A C15 C16 C17 179.5(11) . . . . ?
C15 C16 C17 C18 0.7(8) . . . . ?
C15 C16 C17 C21 -177.4(5) . . . . ?
C14 C13 C18 C17 -1.0(8) . . . . ?
C19 C13 C18 C17 -178.5(5) . . . . ?
C16 C17 C18 C13 -0.1(8) . . . . ?
C21 C17 C18 C13 178.0(5) . . . . ?
Zn2 O5 C19 O6 -7.8(14) . . . . ?
Zn2 O5 C19 C13 175.7(6) . . . . ?
Zn1 O6 C19 O5 7.1(13) . . . . ?
Zn1 O6 C19 C13 -176.4(5) . . . . ?
C18 C13 C19 O5 -3.7(9) . . . . ?
C14 C13 C19 O5 178.8(6) . . . . ?
C18 C13 C19 O6 179.5(6) . . . . ?
C14 C13 C19 O6 2.0(9) . . . . ?
Zn3 O7A C20A O8A 2(2) . . . . ?
Zn3 O7A C20A C15 -178.0(17) . . . . ?
Zn3 O8A C20A O7A -2(2) . . . . ?
Zn3 O8A C20A C15 177.7(16) . . . . ?
C14 C15 C20A O7A -169.2(18) . . . . ?
C16 C15 C20A O7A 11(3) . . . . ?
C20B C15 C20A O7A 18(2) . . . . ?
C14 C15 C20A O8A 11(3) . . . . ?
C16 C15 C20A O8A -168.4(16) . . . . ?
C20B C15 C20A O8A -161(5) . . . . ?
Zn3 O8B C20B O7B -5(5) . . . . ?
Zn3 O8B C20B C15 178.0(12) . . . . ?
C14 C15 C20B O8B -9(4) . . . . ?
C16 C15 C20B O8B 176.6(19) . . . . ?
C20A C15 C20B O8B 2(2) . . . . ?
C14 C15 C20B O7B 174(2) . . . . ?
C16 C15 C20B O7B 0(4) . . . . ?
C20A C15 C20B O7B -174(6) . . . . ?
C16 C17 C21 C25 -74.8(8) . . . . ?
C18 C17 C21 C25 107.1(7) . . . . ?
C16 C17 C21 C22 101.8(7) . . . . ?
C18 C17 C21 C22 -76.3(8) . . . . ?
C25 C21 C22 C25 -3.7(11) . . . 5_764 ?
C17 C21 C22 C25 179.5(7) . . . 5_764 ?
C25 C21 C22 C23 178.0(7) . . . . ?
C17 C21 C22 C23 1.2(10) . . . . ?
C25 C22 C23 C24 0.0(12) 5_764 . . . ?
C21 C22 C23 C24 178.3(8) . . . . ?
C22 C23 C24 C27 2.3(14) . . . 5_764 ?
C22 C21 C25 C22 3.7(11) . . . 5_764 ?
C17 C21 C25 C22 -179.7(7) . . . 5_764 ?
C22 C21 C25 C26 177.9(7) . . . . ?
C17 C21 C25 C26 -5.5(10) . . . . ?
C22 C25 C26 C27 -5.0(13) 5_764 . . . ?
C21 C25 C26 C27 -179.4(8) . . . . ?
C25 C26 C27 C24 2.9(16) . . . 5_764 ?
Zn3 O12 C28 N1 -172.0(10) . . . . ?
C29 N1 C28 O12 7(3) . . . . ?
C30 N1 C28 O12 169.9(18) . . . . ?
Zn3 O13 C31 N2 180.000(2) . . . . ?
C32 N2 C31 O13 180.000(3) . . . . ?
C33 N2 C31 O13 38.4(13) . . . . ?

_refine_diff_density_max         1.510
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.122

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 988120'
#######################################################################
#
#                 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_KT0219

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H26 N1.33 O10.67 Zn2, 6(C3 H7 N O)'
_chemical_formula_sum            'C52 H68 N7.33 O16.67 Zn2'
_chemical_formula_weight         1193.21

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'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   18.5127(3)
_cell_length_b                   18.5127(3)
_cell_length_c                   78.4908(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     23296.4(9)
_cell_formula_units_Z            18
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9435
_cell_measurement_theta_min      2.8083
_cell_measurement_theta_max      66.8075

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_F_000             11244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.826
_shelx_estimated_absorpt_T_min   0.784
_shelx_estimated_absorpt_T_max   0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64531
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      123.0
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_detector_area_resol_mean 10.3389
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            28882
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -90
_diffrn_reflns_limit_l_max       93
_diffrn_reflns_theta_min         2.977
_diffrn_reflns_theta_max         67.050
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             4615
_reflns_number_gt                3739
_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       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

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 -0.037 0.285 0.003 10319 4422 ' '
_platon_squeeze_details          
;
 Squeeze results suggest 6 DMF molecules per formula unit.
 These solvent molecules are included in the formula.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1530P)²+56.7914P]
 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         4615
_refine_ls_number_parameters     224
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0922
_refine_ls_wR_factor_ref         0.2281
_refine_ls_wR_factor_gt          0.2160
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.027
_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 0.54303(3) 0.05514(3) 0.26546(2) 0.0390(3) Uani 1 1 d . . . . .
O1 O 0.4250(2) 0.3919(2) 0.22912(4) 0.0579(8) Uani 1 1 d . . . . .
O2 O 0.4687(2) 0.3508(2) 0.25186(4) 0.0583(8) Uani 1 1 d . . . . .
O3 O 0.4487(2) 0.0211(2) 0.22555(4) 0.0575(8) Uani 1 1 d . . . . .
O4 O 0.4890(2) 0.1004(2) 0.24904(4) 0.0568(8) Uani 1 1 d . . . . .
O5 O 0.5847(3) 0.1315(2) 0.28523(5) 0.0862(13) Uani 1 1 d D . . . .
O6 O 0.6304(9) 0.2207(9) 0.2025(2) 0.092(4) Uiso 0.3333 1 d . . P . .
N1 N 0.6092(3) 0.23932(7) 0.30110(6) 0.196(15) Uiso 0.3333 1 d D . P . .
N2 N 0.6667 0.3333 0.22344(18) 0.107(3) Uiso 1 3 d S . P . .
C1 C 0.4205(3) 0.2623(3) 0.22805(6) 0.0501(10) Uani 1 1 d . . . . .
C2 C 0.4399(3) 0.2068(3) 0.23569(6) 0.0498(10) Uani 1 1 d . . . . .
H2 H 0.4591 0.2154 0.2471 0.060 Uiso 1 1 calc R U . . .
C3 C 0.4311(3) 0.1385(3) 0.22659(6) 0.0476(10) Uani 1 1 d . . . . .
C4 C 0.4022(3) 0.1256(3) 0.20996(6) 0.0504(10) Uani 1 1 d . . . . .
H4 H 0.3957 0.0785 0.2038 0.061 Uiso 1 1 calc R U . . .
C5 C 0.3825(3) 0.1811(3) 0.20212(6) 0.0478(10) Uani 1 1 d . . . . .
C6 C 0.3920(3) 0.2497(3) 0.21166(6) 0.0540(11) Uani 1 1 d . . . . .
H6 H 0.3783 0.2880 0.2066 0.065 Uiso 1 1 calc R U . . .
C7 C 0.4392(3) 0.3416(3) 0.23711(6) 0.0518(10) Uani 1 1 d . . . . .
C8 C 0.4582(3) 0.0822(3) 0.23442(6) 0.0497(10) Uani 1 1 d . . . . .
C9 C 0.3572(3) 0.1717(3) 0.18397(6) 0.0501(10) Uani 1 1 d . . . . .
C10 C 0.4146(3) 0.1849(2) 0.17105(6) 0.0477(10) Uani 1 1 d . . . . .
C11 C 0.4983(3) 0.2052(3) 0.17477(7) 0.0592(12) Uani 1 1 d . . . . .
H11 H 0.5154 0.2093 0.1863 0.071 Uiso 1 1 calc R U . . .
C12 C 0.5540(3) 0.2187(3) 0.16203(7) 0.0645(13) Uani 1 1 d . . . . .
H12 H 0.6088 0.2308 0.1648 0.077 Uiso 1 1 calc R U . . .
C13 C 0.2757(3) 0.1532(2) 0.17977(6) 0.0477(10) Uani 1 1 d . . . . .
C14 C 0.2142(3) 0.1367(3) 0.19257(7) 0.0596(12) Uani 1 1 d . . . . .
H14 H 0.2289 0.1387 0.2042 0.072 Uiso 1 1 calc R U . . .
C15 C 0.1353(3) 0.1182(3) 0.18851(7) 0.0678(14) Uani 1 1 d . . . . .
H15 H 0.0958 0.1078 0.1973 0.081 Uiso 1 1 calc R U . . .
C16A C 0.6293(3) 0.2070(2) 0.28612(6) 0.078(9) Uiso 0.1667 1 d D . P A 1
C16B C 0.5535(3) 0.1531(2) 0.29635(10) 0.072(8) Uiso 0.1667 1 d D . P A 2
C17A C 0.5553(8) 0.2209(8) 0.31690(13) 0.087 Uiso 0.1667 1 d D U P A 1
C17B C 0.6948(6) 0.2959(9) 0.2934(2) 0.087 Uiso 0.1667 1 d D U P A 2
C18A C 0.6667 0.3333 0.30147(19) 0.087 Uiso 0.5 3 d DS U P A 1
C18B C 0.5985(9) 0.2938(8) 0.31418(12) 0.087 Uiso 0.1667 1 d D U P A 2
C19 C 0.6348(11) 0.2445(11) 0.2170(3) 0.136(5) Uiso 0.6667 1 d . . P . .
C20 C 0.6667 0.3333 0.24129(15) 0.073(2) Uiso 1 3 d S . 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
Zn1 O5 1.977(3) . ?
Zn1 O3 2.010(3) 4 ?
Zn1 O2 2.017(3) 2_655 ?
Zn1 O1 2.042(3) 5_655 ?
Zn1 O4 2.050(3) . ?
Zn1 Zn1 3.0027(9) 4 ?
O1 C7 1.254(6) . ?
O1 Zn1 2.042(3) 5_665 ?
O2 C7 1.255(6) . ?
O2 Zn1 2.017(3) 3_665 ?
O3 C8 1.264(6) . ?
O3 Zn1 2.010(3) 4 ?
O4 C8 1.250(6) . ?
O5 C16B 1.2200(10) . ?
O5 C16A 1.2199(10) . ?
O6 C19 1.21(2) . ?
N1 C17B 1.433(13) 3_665 ?
N1 C16B 1.4499(10) . ?
N1 C16A 1.4499(10) . ?
N1 C18B 1.5200(10) . ?
N1 C17A 1.5200(10) . ?
N1 C17B 1.5200(11) . ?
N1 C18A 1.5201(10) . ?
N1 C18B 1.890(12) 2_655 ?
N2 C20 1.401(18) . ?
N2 C19 1.529(19) . ?
N2 C19 1.529(19) 2_655 ?
N2 C19 1.529(19) 3_665 ?
C1 C6 1.365(7) . ?
C1 C2 1.383(6) . ?
C1 C7 1.507(6) . ?
C2 C3 1.390(6) . ?
C3 C4 1.386(6) . ?
C3 C8 1.495(6) . ?
C4 C5 1.394(6) . ?
C5 C6 1.408(7) . ?
C5 C9 1.482(7) . ?
C9 C10 1.401(7) . ?
C9 C13 1.409(7) . ?
C10 C11 1.429(7) . ?
C10 C13 1.429(7) 25 ?
C11 C12 1.367(8) . ?
C12 C15 1.405(8) 25 ?
C13 C10 1.429(7) 25 ?
C13 C14 1.432(7) . ?
C14 C15 1.361(8) . ?
C15 C12 1.406(8) 25 ?
C17B N1 1.433(13) 2_655 ?
C17B C18B 1.639(19) 2_655 ?
C17B C17B 1.83(3) 3_665 ?
C17B C17B 1.83(3) 2_655 ?
C18A N1 1.5201(10) 2_655 ?
C18A N1 1.5201(10) 3_665 ?
C18B C17B 1.639(19) 3_665 ?
C18B N1 1.890(12) 3_665 ?
C18B C18B 1.90(3) 2_655 ?
C18B C18B 1.90(3) 3_665 ?

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
O5 Zn1 O3 97.15(16) . 4 ?
O5 Zn1 O2 94.79(16) . 2_655 ?
O3 Zn1 O2 167.93(14) 4 2_655 ?
O5 Zn1 O1 104.05(16) . 5_655 ?
O3 Zn1 O1 89.78(16) 4 5_655 ?
O2 Zn1 O1 88.99(15) 2_655 5_655 ?
O5 Zn1 O4 107.28(16) . . ?
O3 Zn1 O4 86.76(14) 4 . ?
O2 Zn1 O4 88.06(15) 2_655 . ?
O1 Zn1 O4 148.66(14) 5_655 . ?
O5 Zn1 Zn1 177.10(13) . 4 ?
O3 Zn1 Zn1 85.74(10) 4 4 ?
O2 Zn1 Zn1 82.31(10) 2_655 4 ?
O1 Zn1 Zn1 76.12(9) 5_655 4 ?
O4 Zn1 Zn1 72.57(10) . 4 ?
C7 O1 Zn1 130.6(3) . 5_665 ?
C7 O2 Zn1 123.7(3) . 3_665 ?
C8 O3 Zn1 119.9(3) . 4 ?
C8 O4 Zn1 135.8(3) . . ?
C16B O5 Zn1 135.8(4) . . ?
C16A O5 Zn1 131.6(3) . . ?
C17B N1 C16B 120.7(8) 3_665 . ?
C17B N1 C18B 67.4(8) 3_665 . ?
C16B N1 C18B 130.4(6) . . ?
C16A N1 C17A 147.6(6) . . ?
C17B N1 C17B 76.3(15) 3_665 . ?
C16B N1 C17B 125.4(6) . . ?
C18B N1 C17B 104.27(10) . . ?
C16A N1 C18A 108.1(6) . . ?
C17A N1 C18A 104.28(9) . . ?
C17B N1 C18B 98.8(3) 3_665 2_655 ?
C16B N1 C18B 140.3(6) . 2_655 ?
C18B N1 C18B 66.8(8) . 2_655 ?
C17B N1 C18B 56.2(7) . 2_655 ?
C20 N2 C19 109.4(9) . . ?
C20 N2 C19 109.4(9) . 2_655 ?
C19 N2 C19 109.6(9) . 2_655 ?
C20 N2 C19 109.4(9) . 3_665 ?
C19 N2 C19 109.6(9) . 3_665 ?
C19 N2 C19 109.6(9) 2_655 3_665 ?
C6 C1 C2 120.2(4) . . ?
C6 C1 C7 119.5(4) . . ?
C2 C1 C7 120.0(4) . . ?
C1 C2 C3 119.9(4) . . ?
C4 C3 C2 120.0(4) . . ?
C4 C3 C8 120.2(4) . . ?
C2 C3 C8 119.7(4) . . ?
C3 C4 C5 120.7(4) . . ?
C4 C5 C6 118.0(4) . . ?
C4 C5 C9 121.4(4) . . ?
C6 C5 C9 120.4(4) . . ?
C1 C6 C5 121.2(4) . . ?
O1 C7 O2 126.8(4) . . ?
O1 C7 C1 117.1(4) . . ?
O2 C7 C1 116.1(4) . . ?
O4 C8 O3 125.9(4) . . ?
O4 C8 C3 117.2(4) . . ?
O3 C8 C3 116.9(4) . . ?
C10 C9 C13 120.0(5) . . ?
C10 C9 C5 120.5(4) . . ?
C13 C9 C5 119.4(4) . . ?
C9 C10 C11 121.8(5) . . ?
C9 C10 C13 120.1(4) . 25 ?
C11 C10 C13 118.1(4) . 25 ?
C12 C11 C10 121.2(5) . . ?
C11 C12 C15 120.9(5) . 25 ?
C9 C13 C10 119.9(5) . 25 ?
C9 C13 C14 121.8(5) . . ?
C10 C13 C14 118.3(4) 25 . ?
C15 C14 C13 121.9(5) . . ?
C14 C15 C12 119.6(5) . 25 ?
O5 C16A N1 110.70(12) . . ?
O5 C16B N1 110.69(12) . . ?
N1 C17B N1 126.1(9) 2_655 . ?
N1 C17B C18B 58.8(6) 2_655 2_655 ?
N1 C17B C18B 73.4(7) . 2_655 ?
N1 C17B C17B 107.8(9) 2_655 3_665 ?
N1 C17B C17B 49.7(8) . 3_665 ?
C18B C17B C17B 94.1(9) 2_655 3_665 ?
N1 C17B C17B 54.0(9) 2_655 2_655 ?
N1 C17B C17B 104.0(6) . 2_655 ?
C18B C17B C17B 87.5(9) 2_655 2_655 ?
C17B C17B C17B 59.998(8) 3_665 2_655 ?
N1 C18A N1 119.96(5) 2_655 . ?
N1 C18A N1 119.96(5) 2_655 3_665 ?
N1 C18A N1 119.96(5) . 3_665 ?
N1 C18B C17B 53.8(4) . 3_665 ?
N1 C18B N1 100.5(5) . 3_665 ?
C17B C18B N1 50.4(4) 3_665 3_665 ?
N1 C18B C18B 66.0(5) . 2_655 ?
C17B C18B C18B 91.4(9) 3_665 2_655 ?
N1 C18B C18B 95.1(5) 3_665 2_655 ?
N1 C18B C18B 109.2(5) . 3_665 ?
C17B C18B C18B 85.0(8) 3_665 3_665 ?
N1 C18B C18B 47.3(5) 3_665 3_665 ?
C18B C18B C18B 60.001(7) 2_655 3_665 ?
O6 C19 N2 128.6(17) . . ?

_refine_diff_density_max         1.027
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.106

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 988121'
#######################################################################
#
#                 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_KT0218

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H18 O10 Zn2, 1.5(C3 H7 N O)'
_chemical_formula_sum            'C34.50 H28.50 N1.50 O11.50 Zn2'
_chemical_formula_weight         778.83

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      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'

_cell_length_a                   27.063(9)
_cell_length_b                   27.063(9)
_cell_length_c                   16.107(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10216(7)
_cell_formula_units_Z            9
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    71879
_cell_measurement_theta_min      2.607
_cell_measurement_theta_max      30.956

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_F_000             3582
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.104
_shelx_estimated_absorpt_T_min   0.947
_shelx_estimated_absorpt_T_max   0.957
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Australian Synchrotron'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            71870
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.607
_diffrn_reflns_theta_max         30.956
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             3753
_reflns_number_gt                3455
_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_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

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 0.000 0.000 -0.004 1699 203 ' '
2 0.333 0.667 0.272 1697 202 ' '
3 0.667 0.333 0.938 1697 202 ' '
_platon_squeeze_details          
;
 Squeeze suggests 1.5 DMF molecules per formula unit.
 These solvent molecules are included in the formula.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0815P)²+42.6837P]
 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         3753
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0690
_refine_ls_wR_factor_ref         0.1954
_refine_ls_wR_factor_gt          0.1920
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_restrained_S_all      1.177
_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 0.13443(2) 0.26886(2) 0.34117(3) 0.03470(18) Uani 1 2 d S T P . .
O1 O 0.19512(11) 0.28390(14) 0.25573(19) 0.0616(7) Uani 1 1 d . . . . .
O2 O 0.24271(13) 0.37919(14) 0.2422(2) 0.0641(8) Uani 1 1 d . . . . .
O7 O 0.09245(8) 0.18491(16) 0.3448(4) 0.0778(14) Uani 1 2 d S T P . .
C1 C 0.3333 0.3766(2) 0.1667 0.0446(9) Uani 1 2 d S T P . .
H1 H 0.3333 0.4117 0.1667 0.053 Uiso 1 2 calc R U P . .
C2 C 0.28670(13) 0.32749(16) 0.1964(2) 0.0445(7) Uani 1 1 d . . . . .
C3 C 0.28620(13) 0.27624(16) 0.1954(2) 0.0453(7) Uani 1 1 d . . . . .
H3 H 0.2534 0.2426 0.2144 0.054 Uiso 1 1 calc R U . . .
C4 C 0.3333 0.27329(19) 0.1667 0.0432(9) Uani 1 2 d S T P . .
C5 C 0.23715(15) 0.3307(2) 0.2336(2) 0.0524(8) Uani 1 1 d . . . . .
C6 C 0.3333 0.21845(19) 0.1667 0.0433(9) Uani 1 2 d S T P . .
C7 C 0.31263(15) 0.18280(15) 0.0976(2) 0.0460(7) Uani 1 1 d . . . . .
C8 C 0.29101(19) 0.1971(2) 0.0247(2) 0.0579(9) Uani 1 1 d . . . . .
H8 H 0.2906 0.2320 0.0233 0.069 Uiso 1 1 calc R U . . .
C9 C 0.2715(2) 0.1618(2) -0.0414(3) 0.0712(12) Uani 1 1 d . . . . .
H9 H 0.2576 0.1722 -0.0885 0.085 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 O7 1.969(4) . ?
Zn1 O2 2.014(3) 31 ?
Zn1 O2 2.015(3) 16 ?
Zn1 O1 2.022(3) . ?
Zn1 O1 2.022(3) 22 ?
Zn1 Zn1 3.0324(13) 31 ?
O1 C5 1.258(5) . ?
O2 C5 1.252(5) . ?
O2 Zn1 2.014(3) 31 ?
C1 C2 1.383(4) . ?
C1 C2 1.383(4) 11 ?
C1 H1 0.9500 . ?
C2 C3 1.380(5) . ?
C2 C5 1.509(5) . ?
C3 C4 1.396(4) . ?
C3 H3 0.9500 . ?
C4 C3 1.396(4) 11 ?
C4 C6 1.484(7) . ?
C6 C7 1.393(4) 11 ?
C6 C7 1.393(4) . ?
C7 C7 1.433(7) 23 ?
C7 C8 1.449(5) . ?
C8 C9 1.349(6) . ?
C8 H8 0.9500 . ?
C9 C9 1.411(11) 23 ?
C9 H9 0.9500 . ?

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
O7 Zn1 O2 101.33(15) . 31 ?
O7 Zn1 O2 101.33(15) . 16 ?
O2 Zn1 O2 91.1(2) 31 16 ?
O7 Zn1 O1 101.22(15) . . ?
O2 Zn1 O1 157.45(14) 31 . ?
O2 Zn1 O1 84.71(13) 16 . ?
O7 Zn1 O1 101.22(16) . 22 ?
O2 Zn1 O1 84.72(13) 31 22 ?
O2 Zn1 O1 157.45(14) 16 22 ?
O1 Zn1 O1 90.74(17) . 22 ?
O7 Zn1 Zn1 176.94(18) . 31 ?
O2 Zn1 Zn1 80.78(10) 31 31 ?
O2 Zn1 Zn1 80.78(10) 16 31 ?
O1 Zn1 Zn1 76.68(10) . 31 ?
O1 Zn1 Zn1 76.68(10) 22 31 ?
C5 O1 Zn1 129.1(3) . . ?
C5 O2 Zn1 124.0(3) . 31 ?
C2 C1 C2 119.3(5) . 11 ?
C2 C1 H1 120.3 . . ?
C2 C1 H1 120.3 11 . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 C5 120.0(3) . . ?
C1 C2 C5 119.5(4) . . ?
C2 C3 C4 120.8(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C3 118.1(5) . 11 ?
C3 C4 C6 120.9(2) . . ?
C3 C4 C6 120.9(2) 11 . ?
O2 C5 O1 126.7(3) . . ?
O2 C5 C2 117.3(4) . . ?
O1 C5 C2 115.9(4) . . ?
C7 C6 C7 121.1(5) 11 . ?
C7 C6 C4 119.4(2) 11 . ?
C7 C6 C4 119.4(2) . . ?
C6 C7 C7 119.4(2) . 23 ?
C6 C7 C8 122.6(4) . . ?
C7 C7 C8 118.0(2) 23 . ?
C9 C8 C7 121.2(4) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C9 120.8(3) . 23 ?
C8 C9 H9 119.6 . . ?
C9 C9 H9 119.6 23 . ?

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
C2 C1 C2 C3 -1.0(2) 11 . . . ?
C2 C1 C2 C5 176.5(3) 11 . . . ?
C1 C2 C3 C4 1.9(5) . . . . ?
C5 C2 C3 C4 -175.5(3) . . . . ?
C2 C3 C4 C3 -1.0(2) . . . 11 ?
C2 C3 C4 C6 179.0(2) . . . . ?
Zn1 O2 C5 O1 21.1(6) 31 . . . ?
Zn1 O2 C5 C2 -155.9(3) 31 . . . ?
Zn1 O1 C5 O2 -21.0(6) . . . . ?
Zn1 O1 C5 C2 156.0(2) . . . . ?
C3 C2 C5 O2 171.5(4) . . . . ?
C1 C2 C5 O2 -5.9(5) . . . . ?
C3 C2 C5 O1 -5.8(5) . . . . ?
C1 C2 C5 O1 176.8(3) . . . . ?
C3 C4 C6 C7 -90.8(2) . . . 11 ?
C3 C4 C6 C7 89.2(2) 11 . . 11 ?
C3 C4 C6 C7 89.2(2) . . . . ?
C3 C4 C6 C7 -90.8(2) 11 . . . ?
C7 C6 C7 C7 -0.004(1) 11 . . 23 ?
C4 C6 C7 C7 180.000(1) . . . 23 ?
C7 C6 C7 C8 -179.8(4) 11 . . . ?
C4 C6 C7 C8 0.2(4) . . . . ?
C6 C7 C8 C9 179.7(4) . . . . ?
C7 C7 C8 C9 -0.1(5) 23 . . . ?
C7 C8 C9 C9 0.1(5) . . . 23 ?

_refine_diff_density_max         0.875
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.092

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 988122'
