# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Biao Wu'
_publ_contact_author_email       WUBIAO@LZB.AC.CN

_publ_section_title              
;
Metallomacrocycle or helix: Supramolecular isomerism
in bis(pyridylurea) metal complexes
;
loop_
_publ_author_name
'Biao Wu'
'Chuandong Jia'
'Jianjun Liang'
'Xiao-Juan Yang'

# Attachment 'ZnL-TXH.cif'

data_ZnLtoluene
_database_code_depnum_ccdc_archive 'CCDC 704561'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H48 Cl4 N12 O4 Zn2'
_chemical_formula_weight         1021.43

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'
Cl Cl 0.1484 0.1585 '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           Orthorhombic
_symmetry_space_group_name_H-M   Aba2

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

_cell_length_a                   12.9497(8)
_cell_length_b                   41.020(3)
_cell_length_c                   8.8874(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4721.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2422
_cell_measurement_theta_min      2.82
_cell_measurement_theta_max      21.86

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2104
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13347
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         26.82
_reflns_number_total             4468
_reflns_number_gt                2897
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0440P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(17)
_refine_ls_number_reflns         4468
_refine_ls_number_parameters     281
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1129
_refine_ls_wR_factor_gt          0.0968
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.97438(4) 0.179577(12) 0.41474(8) 0.05063(18) Uani 1 1 d . . .
Cl1 Cl 0.93116(12) 0.22356(3) 0.28662(18) 0.0746(4) Uani 1 1 d . . .
Cl2 Cl 0.94322(10) 0.13219(3) 0.29568(17) 0.0606(4) Uani 1 1 d . . .
N1 N 0.9156(3) 0.17630(10) 0.6293(5) 0.0510(11) Uani 1 1 d . . .
N2 N 0.8123(3) 0.11322(8) 0.8818(4) 0.0459(10) Uani 1 1 d . . .
H2A H 0.8135 0.1105 0.9777 0.055 Uiso 1 1 calc R . .
N3 N 0.7356(3) 0.06329(8) 0.8750(5) 0.0547(12) Uani 1 1 d . . .
H3B H 0.7361 0.0641 0.9717 0.066 Uiso 1 1 calc R . .
N4 N 0.6664(4) -0.08622(11) 0.8153(7) 0.0739(14) Uani 1 1 d . . .
H4B H 0.6029 -0.0921 0.8250 0.089 Uiso 1 1 calc R . .
N5 N 0.6811(3) -0.13007(10) 0.6594(5) 0.0597(13) Uani 1 1 d . . .
H5B H 0.6152 -0.1311 0.6704 0.072 Uiso 1 1 calc R . .
N6 N 0.8699(3) -0.18066(9) 0.4593(5) 0.0512(12) Uani 1 1 d . . .
O1 O 0.7796(3) 0.08838(8) 0.6577(4) 0.0587(10) Uani 1 1 d . . .
O2 O 0.8217(3) -0.09892(9) 0.7182(5) 0.0730(12) Uani 1 1 d . . .
C1 C 0.8825(4) 0.14733(12) 0.6797(6) 0.0481(13) Uani 1 1 d . . .
H1A H 0.8821 0.1296 0.6146 0.058 Uiso 1 1 calc R . .
C2 C 0.8489(3) 0.14320(11) 0.8270(6) 0.0404(11) Uani 1 1 d . . .
C3 C 0.8513(4) 0.16968(11) 0.9205(8) 0.0546(12) Uani 1 1 d . . .
H3A H 0.8289 0.1677 1.0195 0.066 Uiso 1 1 calc R . .
C4 C 0.8868(5) 0.19923(13) 0.8683(7) 0.0677(18) Uani 1 1 d . . .
H4A H 0.8906 0.2171 0.9324 0.081 Uiso 1 1 calc R . .
C5 C 0.9163(5) 0.20199(13) 0.7218(7) 0.0621(15) Uani 1 1 d . . .
H5A H 0.9373 0.2222 0.6853 0.075 Uiso 1 1 calc R . .
C6 C 0.7752(4) 0.08812(11) 0.7983(6) 0.0440(11) Uani 1 1 d . . .
C7 C 0.6911(5) 0.03463(12) 0.8017(7) 0.0685(16) Uani 1 1 d . . .
H7A H 0.7174 0.0331 0.6997 0.082 Uiso 1 1 calc R . .
H7B H 0.6167 0.0371 0.7962 0.082 Uiso 1 1 calc R . .
C8 C 0.7160(4) 0.00406(9) 0.8838(7) 0.0564(15) Uani 1 1 d . . .
H8A H 0.6881 0.0055 0.9849 0.068 Uiso 1 1 calc R . .
H8B H 0.7905 0.0021 0.8923 0.068 Uiso 1 1 calc R . .
C9 C 0.6741(4) -0.02631(11) 0.8087(7) 0.0603(14) Uani 1 1 d . . .
H9A H 0.5995 -0.0246 0.8021 0.072 Uiso 1 1 calc R . .
H9B H 0.7010 -0.0276 0.7071 0.072 Uiso 1 1 calc R . .
C10 C 0.7017(5) -0.05704(11) 0.8918(8) 0.0700(16) Uani 1 1 d . . .
H10A H 0.7761 -0.0581 0.9034 0.084 Uiso 1 1 calc R . .
H10B H 0.6714 -0.0563 0.9916 0.084 Uiso 1 1 calc R . .
C11 C 0.7296(5) -0.10445(12) 0.7298(7) 0.0583(14) Uani 1 1 d . . .
C12 C 0.7251(4) -0.15437(12) 0.5733(6) 0.0528(13) Uani 1 1 d . . .
C13 C 0.8294(4) -0.15655(13) 0.5408(6) 0.0515(13) Uani 1 1 d . . .
H13A H 0.8733 -0.1405 0.5775 0.062 Uiso 1 1 calc R . .
C14 C 0.6613(5) -0.17878(14) 0.5145(7) 0.0704(18) Uani 1 1 d . . .
H14A H 0.5905 -0.1783 0.5325 0.084 Uiso 1 1 calc R . .
C15 C 0.7034(4) -0.20320(13) 0.4306(9) 0.0785(19) Uani 1 1 d . . .
H15A H 0.6613 -0.2195 0.3911 0.094 Uiso 1 1 calc R . .
C16 C 0.8073(4) -0.20382(11) 0.4043(8) 0.0639(14) Uani 1 1 d . . .
H16A H 0.8352 -0.2206 0.3471 0.077 Uiso 1 1 calc R . .
C17 C 1.4965(6) 0.0316(3) 1.397(2) 0.143(4) Uani 1 1 d . . .
C18 C 1.4932(9) 0.0318(6) 1.2439(17) 0.228(12) Uani 1 1 d . . .
H18A H 1.4868 0.0514 1.1919 0.274 Uiso 1 1 calc R . .
C19 C 1.5000 0.0000 1.159(3) 0.242(19) Uani 1 2 d S . .
H19A H 1.5000 0.0000 1.0547 0.290 Uiso 1 2 calc SR . .
C20 C 1.5000 0.0000 1.4776(19) 0.146(6) Uani 1 2 d S . .
H20A H 1.5000 0.0000 1.5823 0.175 Uiso 1 2 calc SR . .
C21 C 1.4904(13) 0.0610(4) 1.4719(19) 0.112(6) Uani 0.50 1 d P . .
H21A H 1.4896 0.0784 1.4000 0.168 Uiso 0.50 1 calc PR . .
H21B H 1.5491 0.0634 1.5370 0.168 Uiso 0.50 1 calc PR . .
H21C H 1.4282 0.0616 1.5307 0.168 Uiso 0.50 1 calc PR . .


_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
Zn N6 2.055(4) 2_755 ?
Zn N1 2.058(4) . ?
Zn Cl1 2.2056(15) . ?
Zn Cl2 2.2498(15) . ?
N1 C5 1.336(6) . ?
N1 C1 1.340(6) . ?
N2 C6 1.357(6) . ?
N2 C2 1.405(5) . ?
N2 H2A 0.8600 . ?
N3 C6 1.328(6) . ?
N3 C7 1.462(6) . ?
N3 H3B 0.8600 . ?
N4 C11 1.345(7) . ?
N4 C10 1.451(6) . ?
N4 H4B 0.8600 . ?
N5 C11 1.375(6) . ?
N5 C12 1.380(6) . ?
N5 H5B 0.8600 . ?
N6 C13 1.334(6) . ?
N6 C16 1.342(6) . ?
N6 Zn 2.055(4) 2_755 ?
O1 C6 1.251(6) . ?
O2 C11 1.218(6) . ?
C1 C2 1.390(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.368(7) . ?
C3 C4 1.377(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.362(8) . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C7 C8 1.486(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.514(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.504(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C13 1.384(7) . ?
C12 C14 1.400(7) . ?
C13 H13A 0.9300 . ?
C14 C15 1.362(8) . ?
C14 H14A 0.9300 . ?
C15 C16 1.366(7) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C17 C18 1.37(2) . ?
C17 C21 1.378(17) . ?
C17 C20 1.479(14) . ?
C18 C19 1.508(19) . ?
C18 H18A 0.9300 . ?
C19 C18 1.508(19) 2_855 ?
C19 H19A 0.9300 . ?
C20 C17 1.479(14) 2_855 ?
C20 H20A 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?

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
N6 Zn N1 100.73(17) 2_755 . ?
N6 Zn Cl1 109.31(12) 2_755 . ?
N1 Zn Cl1 115.97(12) . . ?
N6 Zn Cl2 106.57(11) 2_755 . ?
N1 Zn Cl2 108.24(12) . . ?
Cl1 Zn Cl2 114.74(7) . . ?
C5 N1 C1 119.7(5) . . ?
C5 N1 Zn 121.1(4) . . ?
C1 N1 Zn 119.1(3) . . ?
C6 N2 C2 126.4(4) . . ?
C6 N2 H2A 116.8 . . ?
C2 N2 H2A 116.8 . . ?
C6 N3 C7 122.7(4) . . ?
C6 N3 H3B 118.7 . . ?
C7 N3 H3B 118.7 . . ?
C11 N4 C10 122.1(5) . . ?
C11 N4 H4B 118.9 . . ?
C10 N4 H4B 118.9 . . ?
C11 N5 C12 127.9(5) . . ?
C11 N5 H5B 116.0 . . ?
C12 N5 H5B 116.0 . . ?
C13 N6 C16 119.0(4) . . ?
C13 N6 Zn 118.3(3) . 2_755 ?
C16 N6 Zn 122.6(4) . 2_755 ?
N1 C1 C2 121.5(5) . . ?
N1 C1 H1A 119.2 . . ?
C2 C1 H1A 119.2 . . ?
C3 C2 C1 117.9(5) . . ?
C3 C2 N2 119.5(4) . . ?
C1 C2 N2 122.6(4) . . ?
C2 C3 C4 120.1(6) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C5 C4 C3 119.3(6) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
N1 C5 C4 121.4(5) . . ?
N1 C5 H5A 119.3 . . ?
C4 C5 H5A 119.3 . . ?
O1 C6 N3 122.4(4) . . ?
O1 C6 N2 121.6(4) . . ?
N3 C6 N2 116.0(4) . . ?
N3 C7 C8 112.0(4) . . ?
N3 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N3 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 C9 113.6(4) . . ?
C7 C8 H8A 108.9 . . ?
C9 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
C9 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 C8 112.8(4) . . ?
C10 C9 H9A 109.0 . . ?
C8 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
C8 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
N4 C10 C9 112.7(5) . . ?
N4 C10 H10A 109.0 . . ?
C9 C10 H10A 109.0 . . ?
N4 C10 H10B 109.0 . . ?
C9 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
O2 C11 N4 122.7(5) . . ?
O2 C11 N5 123.5(5) . . ?
N4 C11 N5 113.8(5) . . ?
N5 C12 C13 124.5(5) . . ?
N5 C12 C14 118.6(5) . . ?
C13 C12 C14 116.9(5) . . ?
N6 C13 C12 123.0(5) . . ?
N6 C13 H13A 118.5 . . ?
C12 C13 H13A 118.5 . . ?
C15 C14 C12 119.6(5) . . ?
C15 C14 H14A 120.2 . . ?
C12 C14 H14A 120.2 . . ?
C14 C15 C16 120.1(5) . . ?
C14 C15 H15A 119.9 . . ?
C16 C15 H15A 119.9 . . ?
N6 C16 C15 121.3(5) . . ?
N6 C16 H16A 119.3 . . ?
C15 C16 H16A 119.3 . . ?
C18 C17 C21 118.2(18) . . ?
C18 C17 C20 119.3(16) . . ?
C21 C17 C20 122.4(17) . . ?
C17 C18 C19 119(2) . . ?
C17 C18 H18A 120.3 . . ?
C19 C18 H18A 120.3 . . ?
C18 C19 C18 120(3) 2_855 . ?
C18 C19 H19A 119.9 2_855 . ?
C18 C19 H19A 119.9 . . ?
C17 C20 C17 122.4(18) 2_855 . ?
C17 C20 H20A 118.8 2_855 . ?
C17 C20 H20A 118.8 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 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
N6 Zn N1 C5 73.6(4) 2_755 . . . ?
Cl1 Zn N1 C5 -44.2(5) . . . . ?
Cl2 Zn N1 C5 -174.8(4) . . . . ?
N6 Zn N1 C1 -101.9(4) 2_755 . . . ?
Cl1 Zn N1 C1 140.3(3) . . . . ?
Cl2 Zn N1 C1 9.7(4) . . . . ?
C5 N1 C1 C2 -0.2(7) . . . . ?
Zn N1 C1 C2 175.4(4) . . . . ?
N1 C1 C2 C3 -0.6(7) . . . . ?
N1 C1 C2 N2 178.9(4) . . . . ?
C6 N2 C2 C3 158.2(5) . . . . ?
C6 N2 C2 C1 -21.3(7) . . . . ?
C1 C2 C3 C4 -0.4(7) . . . . ?
N2 C2 C3 C4 -179.9(5) . . . . ?
C2 C3 C4 C5 2.1(9) . . . . ?
C1 N1 C5 C4 1.9(9) . . . . ?
Zn N1 C5 C4 -173.5(5) . . . . ?
C3 C4 C5 N1 -2.9(9) . . . . ?
C7 N3 C6 O1 -1.9(7) . . . . ?
C7 N3 C6 N2 179.1(4) . . . . ?
C2 N2 C6 O1 7.2(7) . . . . ?
C2 N2 C6 N3 -173.8(4) . . . . ?
C6 N3 C7 C8 141.7(5) . . . . ?
N3 C7 C8 C9 -178.2(5) . . . . ?
C7 C8 C9 C10 178.9(5) . . . . ?
C11 N4 C10 C9 99.4(6) . . . . ?
C8 C9 C10 N4 -176.8(5) . . . . ?
C10 N4 C11 O2 4.6(9) . . . . ?
C10 N4 C11 N5 -176.4(5) . . . . ?
C12 N5 C11 O2 3.8(9) . . . . ?
C12 N5 C11 N4 -175.1(5) . . . . ?
C11 N5 C12 C13 -1.2(9) . . . . ?
C11 N5 C12 C14 178.5(6) . . . . ?
C16 N6 C13 C12 0.7(8) . . . . ?
Zn N6 C13 C12 177.9(4) 2_755 . . . ?
N5 C12 C13 N6 178.8(5) . . . . ?
C14 C12 C13 N6 -0.8(8) . . . . ?
N5 C12 C14 C15 -179.3(6) . . . . ?
C13 C12 C14 C15 0.4(9) . . . . ?
C12 C14 C15 C16 0.1(11) . . . . ?
C13 N6 C16 C15 -0.2(9) . . . . ?
Zn N6 C16 C15 -177.3(5) 2_755 . . . ?
C14 C15 C16 N6 -0.2(11) . . . . ?
C21 C17 C18 C19 179.8(10) . . . . ?
C20 C17 C18 C19 -3.8(14) . . . . ?
C17 C18 C19 C18 2.0(7) . . . 2_855 ?
C18 C17 C20 C17 2.0(8) . . . 2_855 ?
C21 C17 C20 C17 178.2(12) . . . 2_855 ?

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
N4 H4B Cl2 0.86 2.66 3.455(5) 155.0 7_445
N5 H5B Cl2 0.86 2.49 3.311(4) 159.9 7_445
N2 H2A O1 0.86 2.20 2.910(5) 139.8 8_645
N3 H3B O1 0.86 1.94 2.723(5) 150.5 8_645
C1 H1A O1 0.93 2.18 2.768(6) 120.1 .
C10 H10B O2 0.97 2.67 3.385(8) 131.0 8_645
C13 H13A O2 0.93 2.22 2.843(6) 124.0 .

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.82
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.069

###################

data_ZnLxylene
_database_code_depnum_ccdc_archive 'CCDC 704562'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H50 Cl4 N12 O4 Zn2'
_chemical_formula_weight         1035.46

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'
Cl Cl 0.1484 0.1585 '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           Orthorhombic
_symmetry_space_group_name_H-M   Aba2

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

_cell_length_a                   12.965(3)
_cell_length_b                   40.535(8)
_cell_length_c                   8.8052(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4627.5(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4382
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      25.02

_exptl_crystal_description       Block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2136
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12546
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_av_sigmaI/netI    0.1821
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         26.32
_reflns_number_total             4283
_reflns_number_gt                1645
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0803P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0031(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_number_reflns         4283
_refine_ls_number_parameters     282
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1485
_refine_ls_wR_factor_gt          0.1111
_refine_ls_goodness_of_fit_ref   0.739
_refine_ls_restrained_S_all      0.739
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn -0.52386(7) -0.17961(2) -0.49514(14) 0.0607(3) Uani 1 1 d . . .
Cl1 Cl -0.5670(2) -0.22348(6) -0.6236(3) 0.0851(8) Uani 1 1 d . . .
Cl2 Cl -0.55172(15) -0.13203(5) -0.6137(3) 0.0714(7) Uani 1 1 d . . .
N1 N -0.5827(5) -0.17680(18) -0.2833(8) 0.0585(19) Uani 1 1 d . . .
N2 N -0.6944(4) -0.11459(15) -0.0317(8) 0.0545(19) Uani 1 1 d . . .
H2A H -0.6970 -0.1130 0.0656 0.065 Uiso 1 1 calc R . .
N3 N -0.7670(5) -0.06401(15) -0.0361(8) 0.065(2) Uani 1 1 d . . .
H3A H -0.7662 -0.0650 0.0614 0.078 Uiso 1 1 calc R . .
N4 N -0.8289(6) 0.08669(18) -0.0940(10) 0.076(2) Uani 1 1 d . . .
H4A H -0.8924 0.0926 -0.0868 0.091 Uiso 1 1 calc R . .
N5 N -0.8163(5) 0.13069(18) -0.2466(9) 0.064(2) Uani 1 1 d . . .
H5A H -0.8819 0.1319 -0.2337 0.077 Uiso 1 1 calc R . .
N6 N -0.6268(6) 0.18098(17) -0.4493(7) 0.060(2) Uani 1 1 d . . .
O1 O -0.7273(5) -0.08920(12) -0.2530(7) 0.0668(18) Uani 1 1 d . . .
O2 O -0.6752(5) 0.09944(16) -0.1929(8) 0.084(2) Uani 1 1 d . . .
C1 C -0.6170(6) -0.1479(2) -0.2346(10) 0.053(2) Uani 1 1 d . . .
H1A H -0.6159 -0.1298 -0.2996 0.064 Uiso 1 1 calc R . .
C2 C -0.6542(6) -0.1442(2) -0.0896(11) 0.052(2) Uani 1 1 d . . .
C3 C -0.6471(6) -0.17064(19) 0.0067(14) 0.065(2) Uani 1 1 d . . .
H3B H -0.6685 -0.1688 0.1071 0.078 Uiso 1 1 calc R . .
C4 C -0.6083(8) -0.1997(2) -0.0458(14) 0.081(3) Uani 1 1 d . . .
H4B H -0.6020 -0.2177 0.0191 0.097 Uiso 1 1 calc R . .
C5 C -0.5787(7) -0.2023(2) -0.1943(14) 0.074(3) Uani 1 1 d . . .
H5B H -0.5556 -0.2224 -0.2317 0.088 Uiso 1 1 calc R . .
C6 C -0.7296(6) -0.0881(2) -0.1111(12) 0.056(2) Uani 1 1 d . . .
C7 C -0.8112(7) -0.0347(2) -0.1079(11) 0.076(3) Uani 1 1 d . . .
H7A H -0.7878 -0.0334 -0.2124 0.091 Uiso 1 1 calc R . .
H7B H -0.8858 -0.0366 -0.1089 0.091 Uiso 1 1 calc R . .
C8 C -0.7820(6) -0.00447(16) -0.0284(11) 0.059(3) Uani 1 1 d . . .
H8A H -0.7073 -0.0028 -0.0270 0.071 Uiso 1 1 calc R . .
H8B H -0.8054 -0.0059 0.0760 0.071 Uiso 1 1 calc R . .
C9 C -0.8256(6) 0.02641(19) -0.0989(11) 0.065(2) Uani 1 1 d . . .
H9A H -0.8013 0.0282 -0.2028 0.078 Uiso 1 1 calc R . .
H9B H -0.9002 0.0248 -0.1015 0.078 Uiso 1 1 calc R . .
C10 C -0.7952(7) 0.05702(18) -0.0131(15) 0.080(3) Uani 1 1 d . . .
H10A H -0.8261 0.0566 0.0871 0.096 Uiso 1 1 calc R . .
H10B H -0.7208 0.0575 -0.0008 0.096 Uiso 1 1 calc R . .
C11 C -0.7650(9) 0.1050(2) -0.1787(12) 0.071(3) Uani 1 1 d . . .
C12 C -0.7709(7) 0.1544(2) -0.3324(11) 0.057(2) Uani 1 1 d . . .
C13 C -0.8342(7) 0.1792(3) -0.3936(12) 0.077(3) Uani 1 1 d . . .
H13A H -0.9053 0.1782 -0.3795 0.093 Uiso 1 1 calc R . .
C14 C -0.7927(8) 0.2041(2) -0.4721(13) 0.080(3) Uani 1 1 d . . .
H14A H -0.8345 0.2210 -0.5082 0.096 Uiso 1 1 calc R . .
C15 C -0.6895(7) 0.20474(19) -0.4991(14) 0.072(2) Uani 1 1 d . . .
H15A H -0.6619 0.2223 -0.5538 0.086 Uiso 1 1 calc R . .
C16 C -0.6694(7) 0.1570(2) -0.3654(11) 0.065(3) Uani 1 1 d . . .
H16A H -0.6257 0.1409 -0.3267 0.078 Uiso 1 1 calc R . .
C17 C 0.0000 0.0000 0.5645(19) 0.086(5) Uani 1 2 d S . .
H17A H 0.0000 0.0000 0.6701 0.103 Uiso 1 2 calc SR . .
C18 C -0.0046(6) -0.0306(3) 0.4913(19) 0.084(3) Uani 1 1 d . . .
C19 C -0.0025(8) -0.0301(4) 0.3269(16) 0.131(6) Uani 1 1 d . . .
H19A H -0.0027 -0.0498 0.2725 0.157 Uiso 1 1 calc R . .
C20 C 0.0000 0.0000 0.251(2) 0.135(9) Uani 1 2 d S . .
H20A H 0.0000 0.0000 0.1455 0.161 Uiso 1 2 calc SR . .
C21 C -0.0041(9) -0.0607(3) 0.5706(16) 0.128(5) Uani 1 1 d . . .
H21A H -0.0055 -0.0565 0.6778 0.192 Uiso 1 1 calc R . .
H21B H 0.0573 -0.0728 0.5455 0.192 Uiso 1 1 calc R . .
H21C H -0.0636 -0.0734 0.5425 0.192 Uiso 1 1 calc R . .


_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
Zn N6 1.996(8) 2_455 ?
Zn N1 2.019(7) . ?
Zn Cl1 2.180(3) . ?
Zn Cl2 2.223(2) . ?
N1 C5 1.297(11) . ?
N1 C1 1.326(9) . ?
N2 C6 1.360(9) . ?
N2 C2 1.403(9) . ?
N2 H2A 0.8600 . ?
N3 C6 1.275(10) . ?
N3 C7 1.463(9) . ?
N3 H3A 0.8600 . ?
N4 C11 1.339(11) . ?
N4 C10 1.464(10) . ?
N4 H4A 0.8600 . ?
N5 C12 1.356(10) . ?
N5 C11 1.372(11) . ?
N5 H5A 0.8600 . ?
N6 C15 1.334(10) . ?
N6 C16 1.340(10) . ?
N6 Zn 1.996(8) 2_455 ?
O1 C6 1.251(11) . ?
O2 C11 1.192(10) . ?
C1 C2 1.373(12) . ?
C1 H1A 0.9300 . ?
C2 C3 1.371(11) . ?
C3 C4 1.361(12) . ?
C3 H3B 0.9300 . ?
C4 C5 1.367(13) . ?
C4 H4B 0.9300 . ?
C5 H5B 0.9300 . ?
C7 C8 1.461(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.507(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.505(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C16 1.352(11) . ?
C12 C13 1.405(11) . ?
C13 C14 1.336(12) . ?
C13 H13A 0.9300 . ?
C14 C15 1.359(10) . ?
C14 H14A 0.9300 . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C17 C18 1.398(14) 2 ?
C17 C18 1.398(14) . ?
C17 H17A 0.9300 . ?
C18 C21 1.407(14) . ?
C18 C19 1.45(2) . ?
C19 C20 1.392(16) . ?
C19 H19A 0.9300 . ?
C20 C19 1.392(16) 2 ?
C20 H20A 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?

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
N6 Zn N1 100.7(3) 2_455 . ?
N6 Zn Cl1 109.5(2) 2_455 . ?
N1 Zn Cl1 115.4(2) . . ?
N6 Zn Cl2 106.2(2) 2_455 . ?
N1 Zn Cl2 108.9(2) . . ?
Cl1 Zn Cl2 114.98(11) . . ?
C5 N1 C1 121.5(8) . . ?
C5 N1 Zn 119.9(7) . . ?
C1 N1 Zn 118.4(6) . . ?
C6 N2 C2 127.8(8) . . ?
C6 N2 H2A 116.1 . . ?
C2 N2 H2A 116.1 . . ?
C6 N3 C7 123.2(8) . . ?
C6 N3 H3A 118.4 . . ?
C7 N3 H3A 118.4 . . ?
C11 N4 C10 122.8(8) . . ?
C11 N4 H4A 118.6 . . ?
C10 N4 H4A 118.6 . . ?
C12 N5 C11 124.8(8) . . ?
C12 N5 H5A 117.6 . . ?
C11 N5 H5A 117.6 . . ?
C15 N6 C16 117.0(8) . . ?
C15 N6 Zn 123.4(6) . 2_455 ?
C16 N6 Zn 119.7(6) . 2_455 ?
N1 C1 C2 121.0(8) . . ?
N1 C1 H1A 119.5 . . ?
C2 C1 H1A 119.5 . . ?
C3 C2 C1 117.8(8) . . ?
C3 C2 N2 118.0(8) . . ?
C1 C2 N2 124.1(8) . . ?
C4 C3 C2 119.5(11) . . ?
C4 C3 H3B 120.3 . . ?
C2 C3 H3B 120.3 . . ?
C3 C4 C5 119.6(10) . . ?
C3 C4 H4B 120.2 . . ?
C5 C4 H4B 120.2 . . ?
N1 C5 C4 120.4(9) . . ?
N1 C5 H5B 119.8 . . ?
C4 C5 H5B 119.8 . . ?
O1 C6 N3 123.6(8) . . ?
O1 C6 N2 118.5(9) . . ?
N3 C6 N2 117.8(9) . . ?
C8 C7 N3 111.8(7) . . ?
C8 C7 H7A 109.2 . . ?
N3 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
N3 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 C9 113.7(7) . . ?
C7 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 C8 112.3(7) . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
N4 C10 C9 110.8(8) . . ?
N4 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
N4 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
O2 C11 N4 123.9(10) . . ?
O2 C11 N5 124.8(10) . . ?
N4 C11 N5 111.3(9) . . ?
C16 C12 N5 126.7(9) . . ?
C16 C12 C13 115.5(9) . . ?
N5 C12 C13 117.8(8) . . ?
C14 C13 C12 120.2(9) . . ?
C14 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
C13 C14 C15 120.2(9) . . ?
C13 C14 H14A 119.9 . . ?
C15 C14 H14A 119.9 . . ?
N6 C15 C14 121.8(9) . . ?
N6 C15 H15A 119.1 . . ?
C14 C15 H15A 119.1 . . ?
N6 C16 C12 125.2(9) . . ?
N6 C16 H16A 117.4 . . ?
C12 C16 H16A 117.4 . . ?
C18 C17 C18 125.1(18) 2 . ?
C18 C17 H17A 117.5 2 . ?
C18 C17 H17A 117.5 . . ?
C17 C18 C21 122.7(15) . . ?
C17 C18 C19 116.7(13) . . ?
C21 C18 C19 120.4(14) . . ?
C20 C19 C18 119.4(16) . . ?
C20 C19 H19A 120.3 . . ?
C18 C19 H19A 120.3 . . ?
C19 C20 C19 123(2) 2 . ?
C19 C20 H20A 118.6 2 . ?
C19 C20 H20A 118.6 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 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
N6 Zn N1 C5 -71.1(7) 2_455 . . . ?
Cl1 Zn N1 C5 46.6(7) . . . . ?
Cl2 Zn N1 C5 177.6(6) . . . . ?
N6 Zn N1 C1 103.4(6) 2_455 . . . ?
Cl1 Zn N1 C1 -139.0(5) . . . . ?
Cl2 Zn N1 C1 -8.0(6) . . . . ?
C5 N1 C1 C2 -3.1(12) . . . . ?
Zn N1 C1 C2 -177.5(6) . . . . ?
N1 C1 C2 C3 5.1(12) . . . . ?
N1 C1 C2 N2 -178.1(7) . . . . ?
C6 N2 C2 C3 -164.0(7) . . . . ?
C6 N2 C2 C1 19.2(12) . . . . ?
C1 C2 C3 C4 -3.0(12) . . . . ?
N2 C2 C3 C4 -179.9(8) . . . . ?
C2 C3 C4 C5 -1.1(14) . . . . ?
C1 N1 C5 C4 -1.2(14) . . . . ?
Zn N1 C5 C4 173.1(7) . . . . ?
C3 C4 C5 N1 3.3(15) . . . . ?
C7 N3 C6 O1 -0.3(13) . . . . ?
C7 N3 C6 N2 -177.4(7) . . . . ?
C2 N2 C6 O1 0.0(12) . . . . ?
C2 N2 C6 N3 177.3(7) . . . . ?
C6 N3 C7 C8 -139.2(8) . . . . ?
N3 C7 C8 C9 179.8(7) . . . . ?
C7 C8 C9 C10 179.2(8) . . . . ?
C11 N4 C10 C9 -100.8(10) . . . . ?
C8 C9 C10 N4 173.6(7) . . . . ?
C10 N4 C11 O2 -2.0(15) . . . . ?
C10 N4 C11 N5 177.8(8) . . . . ?
C12 N5 C11 O2 -3.9(16) . . . . ?
C12 N5 C11 N4 176.3(8) . . . . ?
C11 N5 C12 C16 -0.3(15) . . . . ?
C11 N5 C12 C13 -179.7(9) . . . . ?
C16 C12 C13 C14 -3.2(14) . . . . ?
N5 C12 C13 C14 176.3(9) . . . . ?
C12 C13 C14 C15 3.1(17) . . . . ?
C16 N6 C15 C14 -2.8(15) . . . . ?
Zn N6 C15 C14 176.7(8) 2_455 . . . ?
C13 C14 C15 N6 0.0(18) . . . . ?
C15 N6 C16 C12 2.7(13) . . . . ?
Zn N6 C16 C12 -176.9(7) 2_455 . . . ?
N5 C12 C16 N6 -179.2(8) . . . . ?
C13 C12 C16 N6 0.3(14) . . . . ?
C18 C17 C18 C21 176.8(10) 2 . . . ?
C18 C17 C18 C19 1.2(6) 2 . . . ?
C17 C18 C19 C20 -2.4(13) . . . . ?
C21 C18 C19 C20 -178.1(8) . . . . ?
C18 C19 C20 C19 1.2(7) . . . 2 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.32
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.184

#############

data_ZnLhelix
_database_code_depnum_ccdc_archive 'CCDC 704563'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H20 Cl2 N6 O2 Zn'
_chemical_formula_weight         464.65

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_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                   10.7340(11)
_cell_length_b                   14.3446(11)
_cell_length_c                   13.7280(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.839(2)
_cell_angle_gamma                90.00
_cell_volume                     2043.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2461
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      25.29

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6012
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.42
_diffrn_reflns_theta_max         27.77
_reflns_number_total             2339
_reflns_number_gt                1945
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0365P)²+0.7430P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2339
_refine_ls_number_parameters     123
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0782
_refine_ls_wR_factor_gt          0.0745
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.5000 0.13155(2) 0.2500 0.03889(12) Uani 1 2 d S . .
Cl Cl 0.46947(5) 0.05237(4) 0.10664(4) 0.04949(15) Uani 1 1 d . . .
N1 N 0.34930(16) 0.21876(11) 0.23888(12) 0.0431(4) Uani 1 1 d . . .
N2 N 0.24671(19) 0.38572(14) 0.40482(14) 0.0593(5) Uani 1 1 d . . .
H2A H 0.1864 0.4267 0.3959 0.071 Uiso 1 1 calc R . .
C4 C 0.2536(2) 0.33440(15) 0.32119(15) 0.0461(5) Uani 1 1 d . . .
C5 C 0.3464(2) 0.26713(14) 0.32149(15) 0.0454(5) Uani 1 1 d . . .
H5A H 0.4087 0.2553 0.3811 0.054 Uiso 1 1 calc R . .
C6 C 0.3263(2) 0.37840(17) 0.50157(18) 0.0593(6) Uani 1 1 d . . .
O1 O 0.42052(19) 0.32935(16) 0.52239(13) 0.0903(7) Uani 1 1 d . . .
N3 N 0.28874(19) 0.43211(15) 0.56869(15) 0.0662(6) Uani 1 1 d . . .
H3A H 0.2202 0.4653 0.5491 0.079 Uiso 1 1 calc R . .
C2 C 0.1654(2) 0.29983(18) 0.14725(17) 0.0619(6) Uani 1 1 d . . .
H2B H 0.1033 0.3095 0.0870 0.074 Uiso 1 1 calc R . .
C1 C 0.2597(2) 0.23396(16) 0.15297(16) 0.0541(6) Uani 1 1 d . . .
H1A H 0.2613 0.1993 0.0960 0.065 Uiso 1 1 calc R . .
C3 C 0.1634(2) 0.35090(16) 0.23024(17) 0.0542(6) Uani 1 1 d . . .
H3B H 0.1015 0.3971 0.2262 0.065 Uiso 1 1 calc R . .
C7 C 0.3615(2) 0.43563(19) 0.67429(18) 0.0616(6) Uani 1 1 d . . .
H7A H 0.4032 0.3760 0.6932 0.074 Uiso 1 1 calc R . .
H7B H 0.3023 0.4461 0.7161 0.074 Uiso 1 1 calc R . .
C8 C 0.4611(2) 0.51076(17) 0.69402(18) 0.0643(6) Uani 1 1 d . . .
H8A H 0.4195 0.5708 0.6773 0.077 Uiso 1 1 calc R . .
H8B H 0.5193 0.5014 0.6513 0.077 Uiso 1 1 calc R . .


_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
Zn N1 2.0195(17) 2_655 ?
Zn N1 2.0195(17) . ?
Zn Cl 2.2226(5) . ?
Zn Cl 2.2226(5) 2_655 ?
N1 C1 1.335(2) . ?
N1 C5 1.337(3) . ?
N2 C4 1.382(3) . ?
N2 C6 1.387(3) . ?
C4 C5 1.387(3) . ?
C4 C3 1.390(3) . ?
C6 O1 1.205(3) . ?
C6 N3 1.340(3) . ?
N3 C7 1.461(3) . ?
C2 C3 1.359(3) . ?
C2 C1 1.372(3) . ?
C7 C8 1.493(3) . ?
C8 C8 1.550(5) 2_656 ?

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
N1 Zn N1 103.46(10) 2_655 . ?
N1 Zn Cl 108.48(5) 2_655 . ?
N1 Zn Cl 108.42(5) . . ?
N1 Zn Cl 108.42(5) 2_655 2_655 ?
N1 Zn Cl 108.48(5) . 2_655 ?
Cl Zn Cl 118.53(3) . 2_655 ?
C1 N1 C5 119.80(18) . . ?
C1 N1 Zn 123.34(15) . . ?
C5 N1 Zn 116.71(13) . . ?
C4 N2 C6 127.20(18) . . ?
N2 C4 C5 124.03(18) . . ?
N2 C4 C3 118.86(19) . . ?
C5 C4 C3 117.11(19) . . ?
N1 C5 C4 122.10(18) . . ?
O1 C6 N3 123.7(2) . . ?
O1 C6 N2 123.0(2) . . ?
N3 C6 N2 113.3(2) . . ?
C6 N3 C7 121.6(2) . . ?
C3 C2 C1 119.5(2) . . ?
N1 C1 C2 121.1(2) . . ?
C2 C3 C4 120.3(2) . . ?
N3 C7 C8 112.4(2) . . ?
C7 C8 C8 111.0(2) . 2_656 ?

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
N1 Zn N1 C1 105.67(19) 2_655 . . . ?
Cl Zn N1 C1 -9.37(19) . . . . ?
Cl Zn N1 C1 -139.33(17) 2_655 . . . ?
N1 Zn N1 C5 -69.92(14) 2_655 . . . ?
Cl Zn N1 C5 175.04(13) . . . . ?
Cl Zn N1 C5 45.08(15) 2_655 . . . ?
C6 N2 C4 C5 -1.6(4) . . . . ?
C6 N2 C4 C3 179.0(2) . . . . ?
C1 N1 C5 C4 -0.8(3) . . . . ?
Zn N1 C5 C4 174.92(16) . . . . ?
N2 C4 C5 N1 179.7(2) . . . . ?
C3 C4 C5 N1 -0.9(3) . . . . ?
C4 N2 C6 O1 6.3(5) . . . . ?
C4 N2 C6 N3 -174.6(2) . . . . ?
O1 C6 N3 C7 0.4(4) . . . . ?
N2 C6 N3 C7 -178.7(2) . . . . ?
C5 N1 C1 C2 1.1(3) . . . . ?
Zn N1 C1 C2 -174.32(19) . . . . ?
C3 C2 C1 N1 0.4(4) . . . . ?
C1 C2 C3 C4 -2.2(4) . . . . ?
N2 C4 C3 C2 -178.2(2) . . . . ?
C5 C4 C3 C2 2.4(3) . . . . ?
C6 N3 C7 C8 90.9(3) . . . . ?
N3 C7 C8 C8 -178.4(2) . . . 2_656 ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.049

#########END


