# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compounda-1a
_database_code_depnum_ccdc_archive 'CCDC 1040034'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H26 N4 Ni S2'
_chemical_formula_weight         589.40

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '

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

_cell_length_a                   18.0049(9)
_cell_length_b                   9.0457(4)
_cell_length_c                   32.7494(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5333.8(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4482
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      28.13

_exptl_crystal_description       platelet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2448
_exptl_absorpt_coefficient_mu    0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8383
_exptl_absorpt_correction_T_max  0.9819
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32789
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.24
_diffrn_reflns_theta_max         30.04
_reflns_number_total             7802
_reflns_number_gt                5418
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0625P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7802
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1267
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
C1 C 0.52383(13) 1.0965(3) 0.18525(7) 0.0242(5) Uani 1 1 d . . .
H1 H 0.5350 1.0948 0.1575 0.029 Uiso 1 1 calc R . .
C2 C 0.57547(14) 1.1287(3) 0.21593(7) 0.0274(5) Uani 1 1 d . . .
H2 H 0.6254 1.1517 0.2124 0.033 Uiso 1 1 calc R . .
C3 C 0.53762(14) 1.1197(3) 0.25233(7) 0.0275(5) Uani 1 1 d . . .
H3 H 0.5572 1.1358 0.2782 0.033 Uiso 1 1 calc R . .
C4 C 0.46291(13) 1.0810(3) 0.24303(7) 0.0220(5) Uani 1 1 d . . .
C5 C 0.40585(14) 1.0471(3) 0.27033(7) 0.0211(5) Uani 1 1 d . . .
C6 C 0.33877(13) 0.9829(3) 0.25801(7) 0.0204(5) Uani 1 1 d . . .
C7 C 0.27359(13) 0.9619(3) 0.28173(7) 0.0242(5) Uani 1 1 d . . .
H7 H 0.2677 0.9858 0.3092 0.029 Uiso 1 1 calc R . .
C8 C 0.22070(14) 0.8996(3) 0.25668(7) 0.0265(5) Uani 1 1 d . . .
H8 H 0.1726 0.8724 0.2639 0.032 Uiso 1 1 calc R . .
C9 C 0.25388(13) 0.8858(3) 0.21830(7) 0.0247(5) Uani 1 1 d . . .
H9 H 0.2298 0.8482 0.1954 0.030 Uiso 1 1 calc R . .
C10 C 0.41870(13) 1.0753(3) 0.31438(7) 0.0225(5) Uani 1 1 d . . .
C11 C 0.40624(15) 0.9634(3) 0.34283(7) 0.0249(5) Uani 1 1 d . . .
H11 H 0.3892 0.8718 0.3340 0.030 Uiso 1 1 calc R . .
C12 C 0.41891(15) 0.9862(3) 0.38414(7) 0.0252(5) Uani 1 1 d . . .
H12 H 0.4111 0.9094 0.4025 0.030 Uiso 1 1 calc R . .
C13 C 0.44300(14) 1.1223(3) 0.39814(7) 0.0246(5) Uani 1 1 d . . .
C14 C 0.45701(15) 1.2350(3) 0.36985(7) 0.0281(5) Uani 1 1 d . . .
H14 H 0.4745 1.3261 0.3788 0.034 Uiso 1 1 calc R . .
C15 C 0.44492(15) 1.2115(3) 0.32871(7) 0.0279(5) Uani 1 1 d . . .
H15 H 0.4543 1.2873 0.3102 0.033 Uiso 1 1 calc R . .
C16 C 0.41596(17) 1.0047(3) 0.47519(7) 0.0345(6) Uani 1 1 d . . .
H16A H 0.3656 0.9913 0.4663 0.052 Uiso 1 1 calc R . .
H16B H 0.4168 1.0195 0.5042 0.052 Uiso 1 1 calc R . .
H16C H 0.4445 0.9185 0.4684 0.052 Uiso 1 1 calc R . .
C17 C 0.32379(14) 0.6820(3) 0.15481(7) 0.0238(5) Uani 1 1 d . . .
H17 H 0.3225 0.6603 0.1826 0.029 Uiso 1 1 calc R . .
C18 C 0.30948(15) 0.5790(3) 0.12403(7) 0.0281(5) Uani 1 1 d . . .
H18 H 0.2967 0.4802 0.1275 0.034 Uiso 1 1 calc R . .
C19 C 0.31801(14) 0.6526(3) 0.08780(7) 0.0260(5) Uani 1 1 d . . .
H19 H 0.3122 0.6128 0.0618 0.031 Uiso 1 1 calc R . .
C20 C 0.33723(13) 0.8008(3) 0.09718(7) 0.0202(5) Uani 1 1 d . . .
C21 C 0.35686(13) 0.9131(3) 0.06992(7) 0.0206(5) Uani 1 1 d . . .
C22 C 0.38530(13) 1.0498(3) 0.08213(7) 0.0202(5) Uani 1 1 d . . .
C23 C 0.39510(13) 1.1791(3) 0.05798(7) 0.0227(5) Uani 1 1 d . . .
H23 H 0.3888 1.1862 0.0299 0.027 Uiso 1 1 calc R . .
C24 C 0.41544(15) 1.2908(3) 0.08378(7) 0.0265(5) Uani 1 1 d . . .
H24 H 0.4254 1.3883 0.0766 0.032 Uiso 1 1 calc R . .
C25 C 0.41837(14) 1.2298(3) 0.12307(7) 0.0244(5) Uani 1 1 d . . .
H25 H 0.4305 1.2828 0.1465 0.029 Uiso 1 1 calc R . .
C26 C 0.34731(13) 0.8879(3) 0.02543(7) 0.0221(5) Uani 1 1 d . . .
C27 C 0.27962(14) 0.8446(3) 0.00853(7) 0.0283(6) Uani 1 1 d . . .
H27 H 0.2399 0.8235 0.0257 0.034 Uiso 1 1 calc R . .
C28 C 0.27037(14) 0.8324(3) -0.03337(7) 0.0278(6) Uani 1 1 d . . .
H28 H 0.2248 0.8028 -0.0440 0.033 Uiso 1 1 calc R . .
C29 C 0.32920(14) 0.8643(3) -0.05953(7) 0.0230(5) Uani 1 1 d . . .
C30 C 0.39820(14) 0.9016(3) -0.04310(7) 0.0254(5) Uani 1 1 d . . .
H30 H 0.4385 0.9187 -0.0602 0.030 Uiso 1 1 calc R . .
C31 C 0.40648(13) 0.9130(3) -0.00125(7) 0.0238(5) Uani 1 1 d . . .
H31 H 0.4527 0.9381 0.0094 0.029 Uiso 1 1 calc R . .
C32 C 0.24258(16) 0.7585(4) -0.12342(8) 0.0414(7) Uani 1 1 d . . .
H32A H 0.2481 0.6626 -0.1112 0.062 Uiso 1 1 calc R . .
H32B H 0.2365 0.7481 -0.1524 0.062 Uiso 1 1 calc R . .
H32C H 0.1997 0.8068 -0.1122 0.062 Uiso 1 1 calc R . .
N1 N 0.45602(11) 1.0681(2) 0.20079(5) 0.0201(4) Uani 1 1 d . . .
N2 N 0.32474(11) 0.9332(2) 0.21837(5) 0.0199(4) Uani 1 1 d . . .
N3 N 0.33973(11) 0.8167(2) 0.13955(5) 0.0202(4) Uani 1 1 d . . .
N4 N 0.40133(11) 1.0845(2) 0.12262(5) 0.0219(4) Uani 1 1 d . . .
S1 S 0.45517(4) 1.16350(8) 0.450207(19) 0.03509(17) Uani 1 1 d . . .
S2 S 0.32305(4) 0.86629(8) -0.113169(18) 0.03136(16) Uani 1 1 d . . .
Ni1 Ni 0.379739(17) 0.97554(3) 0.170428(8) 0.01875(9) Uani 1 1 d . . .


_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
C1 N1 1.347(3) . ?
C1 C2 1.400(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.375(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.423(3) . ?
C3 H3 0.9300 . ?
C4 N1 1.394(3) . ?
C4 C5 1.396(3) . ?
C5 C6 1.400(3) . ?
C5 C10 1.483(3) . ?
C6 N2 1.397(3) . ?
C6 C7 1.420(3) . ?
C7 C8 1.377(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.398(3) . ?
C8 H8 0.9300 . ?
C9 N2 1.346(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.394(3) . ?
C10 C15 1.400(3) . ?
C11 C12 1.387(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.384(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.400(3) . ?
C13 S1 1.759(2) . ?
C14 C15 1.381(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 S1 1.797(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N3 1.347(3) . ?
C17 C18 1.397(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.369(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.418(3) . ?
C19 H19 0.9300 . ?
C20 N3 1.396(3) . ?
C20 C21 1.398(3) . ?
C21 C22 1.397(3) . ?
C21 C26 1.485(3) . ?
C22 N4 1.393(3) . ?
C22 C23 1.422(3) . ?
C23 C24 1.367(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.401(3) . ?
C24 H24 0.9300 . ?
C25 N4 1.350(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.395(3) . ?
C26 C31 1.397(3) . ?
C27 C28 1.387(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.392(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.395(3) . ?
C29 S2 1.760(2) . ?
C30 C31 1.383(3) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 S2 1.778(3) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
N1 Ni1 1.8909(19) . ?
N2 Ni1 1.8953(18) . ?
N3 Ni1 1.8992(19) . ?
N4 Ni1 1.8902(19) . ?

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 C1 C2 111.7(2) . . ?
N1 C1 H1 124.1 . . ?
C2 C1 H1 124.1 . . ?
C3 C2 C1 106.3(2) . . ?
C3 C2 H2 126.8 . . ?
C1 C2 H2 126.8 . . ?
C2 C3 C4 107.3(2) . . ?
C2 C3 H3 126.3 . . ?
C4 C3 H3 126.3 . . ?
N1 C4 C5 123.5(2) . . ?
N1 C4 C3 108.5(2) . . ?
C5 C4 C3 127.8(2) . . ?
C4 C5 C6 122.8(2) . . ?
C4 C5 C10 118.0(2) . . ?
C6 C5 C10 119.1(2) . . ?
N2 C6 C5 123.9(2) . . ?
N2 C6 C7 108.4(2) . . ?
C5 C6 C7 127.7(2) . . ?
C8 C7 C6 107.5(2) . . ?
C8 C7 H7 126.3 . . ?
C6 C7 H7 126.3 . . ?
C7 C8 C9 106.1(2) . . ?
C7 C8 H8 127.0 . . ?
C9 C8 H8 127.0 . . ?
N2 C9 C8 112.0(2) . . ?
N2 C9 H9 124.0 . . ?
C8 C9 H9 124.0 . . ?
C11 C10 C15 118.0(2) . . ?
C11 C10 C5 120.0(2) . . ?
C15 C10 C5 122.0(2) . . ?
C12 C11 C10 121.1(2) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C13 C12 C11 120.5(2) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 119.0(2) . . ?
C12 C13 S1 123.28(19) . . ?
C14 C13 S1 117.71(18) . . ?
C15 C14 C13 120.3(2) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C10 121.0(2) . . ?
C14 C15 H15 119.5 . . ?
C10 C15 H15 119.5 . . ?
S1 C16 H16A 109.5 . . ?
S1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C18 112.0(2) . . ?
N3 C17 H17 124.0 . . ?
C18 C17 H17 124.0 . . ?
C19 C18 C17 106.3(2) . . ?
C19 C18 H18 126.9 . . ?
C17 C18 H18 126.9 . . ?
C18 C19 C20 107.4(2) . . ?
C18 C19 H19 126.3 . . ?
C20 C19 H19 126.3 . . ?
N3 C20 C21 123.5(2) . . ?
N3 C20 C19 108.72(19) . . ?
C21 C20 C19 127.6(2) . . ?
C22 C21 C20 123.6(2) . . ?
C22 C21 C26 117.3(2) . . ?
C20 C21 C26 119.1(2) . . ?
N4 C22 C21 123.2(2) . . ?
N4 C22 C23 108.6(2) . . ?
C21 C22 C23 127.9(2) . . ?
C24 C23 C22 107.3(2) . . ?
C24 C23 H23 126.4 . . ?
C22 C23 H23 126.4 . . ?
C23 C24 C25 106.7(2) . . ?
C23 C24 H24 126.7 . . ?
C25 C24 H24 126.7 . . ?
N4 C25 C24 111.4(2) . . ?
N4 C25 H25 124.3 . . ?
C24 C25 H25 124.3 . . ?
C27 C26 C31 117.6(2) . . ?
C27 C26 C21 122.3(2) . . ?
C31 C26 C21 120.0(2) . . ?
C28 C27 C26 121.3(2) . . ?
C28 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C27 C28 C29 120.1(2) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C30 119.4(2) . . ?
C28 C29 S2 124.63(19) . . ?
C30 C29 S2 115.99(18) . . ?
C31 C30 C29 119.7(2) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C26 121.7(2) . . ?
C30 C31 H31 119.1 . . ?
C26 C31 H31 119.1 . . ?
S2 C32 H32A 109.5 . . ?
S2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
S2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C1 N1 C4 106.15(19) . . ?
C1 N1 Ni1 122.95(16) . . ?
C4 N1 Ni1 128.58(16) . . ?
C9 N2 C6 105.99(19) . . ?
C9 N2 Ni1 123.93(15) . . ?
C6 N2 Ni1 127.64(16) . . ?
C17 N3 C20 105.59(19) . . ?
C17 N3 Ni1 124.56(16) . . ?
C20 N3 Ni1 128.28(15) . . ?
C25 N4 C22 106.05(19) . . ?
C25 N4 Ni1 123.04(16) . . ?
C22 N4 Ni1 128.95(16) . . ?
C13 S1 C16 102.89(12) . . ?
C29 S2 C32 103.53(13) . . ?
N4 Ni1 N1 93.17(8) . . ?
N4 Ni1 N2 154.01(9) . . ?
N1 Ni1 N2 91.91(8) . . ?
N4 Ni1 N3 91.80(8) . . ?
N1 Ni1 N3 152.93(9) . . ?
N2 Ni1 N3 95.17(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.04
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.104
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compoundb-1a
_database_code_depnum_ccdc_archive 'CCDC 1040035'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H26 N4 Ni S2'
_chemical_formula_sum            'C32 H26 N4 Ni S2'
_chemical_formula_weight         589.40

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   9.7891(2)
_cell_length_b                   11.7331(2)
_cell_length_c                   12.5712(3)
_cell_angle_alpha                104.4860(10)
_cell_angle_beta                 99.6890(10)
_cell_angle_gamma                102.5310(10)
_cell_volume                     1326.30(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8946
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      29.60

_exptl_crystal_description       prism
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             612
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9137
_exptl_absorpt_correction_T_max  0.9137
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26383
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         29.36
_reflns_number_total             7063
_reflns_number_gt                5967
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0340P)²+1.0976P] 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         7063
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_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
C1 C 0.5379(2) 0.9473(2) 0.73237(17) 0.0278(4) Uani 1 1 d . . .
H1 H 0.5540 1.0302 0.7393 0.033 Uiso 1 1 calc R . .
C2 C 0.4119(2) 0.8739(2) 0.74590(17) 0.0298(4) Uani 1 1 d . . .
H2 H 0.3315 0.8984 0.7620 0.036 Uiso 1 1 calc R . .
C3 C 0.4308(2) 0.7591(2) 0.73074(16) 0.0270(4) Uani 1 1 d . . .
H3 H 0.3654 0.6907 0.7347 0.032 Uiso 1 1 calc R . .
C4 C 0.5693(2) 0.76386(19) 0.70780(15) 0.0239(4) Uani 1 1 d . . .
C5 C 0.6396(2) 0.67124(19) 0.69425(15) 0.0237(4) Uani 1 1 d . . .
C6 C 0.7833(2) 0.69098(19) 0.68574(16) 0.0241(4) Uani 1 1 d . . .
C7 C 0.8546(2) 0.6017(2) 0.64479(17) 0.0294(4) Uani 1 1 d . . .
H7 H 0.8186 0.5174 0.6273 0.035 Uiso 1 1 calc R . .
C8 C 0.9865(2) 0.6632(2) 0.63592(19) 0.0342(5) Uani 1 1 d . . .
H8 H 1.0568 0.6289 0.6107 0.041 Uiso 1 1 calc R . .
C9 C 0.9943(2) 0.7878(2) 0.67230(19) 0.0309(5) Uani 1 1 d . . .
H9 H 1.0729 0.8502 0.6750 0.037 Uiso 1 1 calc R . .
C10 C 0.5599(2) 0.54614(19) 0.68830(16) 0.0250(4) Uani 1 1 d . . .
C11 C 0.6205(2) 0.4830(2) 0.75613(17) 0.0275(4) Uani 1 1 d . . .
H11 H 0.7096 0.5213 0.8065 0.033 Uiso 1 1 calc R . .
C12 C 0.5504(2) 0.3652(2) 0.74952(17) 0.0274(4) Uani 1 1 d . . .
H12 H 0.5926 0.3248 0.7951 0.033 Uiso 1 1 calc R . .
C13 C 0.4162(2) 0.30618(19) 0.67476(16) 0.0254(4) Uani 1 1 d . . .
C14 C 0.3540(2) 0.3682(2) 0.60723(17) 0.0279(4) Uani 1 1 d . . .
H14 H 0.2645 0.3301 0.5573 0.034 Uiso 1 1 calc R . .
C15 C 0.4254(2) 0.4864(2) 0.61451(16) 0.0271(4) Uani 1 1 d . . .
H15 H 0.3828 0.5270 0.5692 0.033 Uiso 1 1 calc R . .
C16 C 0.1626(2) 0.1165(2) 0.58040(19) 0.0334(5) Uani 1 1 d . . .
H16A H 0.1119 0.1753 0.6068 0.050 Uiso 1 1 calc R . .
H16B H 0.1091 0.0368 0.5785 0.050 Uiso 1 1 calc R . .
H16C H 0.1735 0.1159 0.5058 0.050 Uiso 1 1 calc R . .
C17 C 1.0847(2) 1.0029(2) 0.89870(18) 0.0296(4) Uani 1 1 d . . .
H17 H 1.0703 0.9201 0.8917 0.036 Uiso 1 1 calc R . .
C18 C 1.1830(2) 1.0976(2) 0.98824(18) 0.0326(5) Uani 1 1 d . . .
H18 H 1.2437 1.0889 1.0493 0.039 Uiso 1 1 calc R . .
C19 C 1.1721(2) 1.2047(2) 0.96819(17) 0.0285(4) Uani 1 1 d . . .
H19 H 1.2244 1.2830 1.0133 0.034 Uiso 1 1 calc R . .
C20 C 1.0662(2) 1.17494(19) 0.86564(16) 0.0249(4) Uani 1 1 d . . .
C21 C 1.0163(2) 1.25378(19) 0.81127(16) 0.0240(4) Uani 1 1 d . . .
C22 C 0.8965(2) 1.21189(19) 0.71906(16) 0.0249(4) Uani 1 1 d . . .
C23 C 0.8549(2) 1.2724(2) 0.63962(17) 0.0308(5) Uani 1 1 d . . .
H23 H 0.8998 1.3514 0.6410 0.037 Uiso 1 1 calc R . .
C24 C 0.7367(3) 1.1935(2) 0.56067(17) 0.0344(5) Uani 1 1 d . . .
H24 H 0.6861 1.2083 0.4983 0.041 Uiso 1 1 calc R . .
C25 C 0.7069(2) 1.0861(2) 0.59228(17) 0.0299(4) Uani 1 1 d . . .
H25 H 0.6312 1.0172 0.5530 0.036 Uiso 1 1 calc R . .
C26 C 1.0900(2) 1.38622(19) 0.85261(16) 0.0259(4) Uani 1 1 d . . .
C27 C 1.2396(2) 1.4316(2) 0.88114(17) 0.0287(4) Uani 1 1 d . . .
H27 H 1.2961 1.3774 0.8702 0.034 Uiso 1 1 calc R . .
C28 C 1.3056(2) 1.5562(2) 0.92549(18) 0.0308(4) Uani 1 1 d . . .
H28 H 1.4055 1.5846 0.9444 0.037 Uiso 1 1 calc R . .
C29 C 1.2223(2) 1.6390(2) 0.94184(17) 0.0285(4) Uani 1 1 d . . .
C30 C 1.0729(2) 1.5949(2) 0.90931(17) 0.0293(4) Uani 1 1 d . . .
H30 H 1.0164 1.6494 0.9168 0.035 Uiso 1 1 calc R . .
C31 C 1.0082(2) 1.4711(2) 0.86608(17) 0.0281(4) Uani 1 1 d . . .
H31 H 0.9082 1.4432 0.8454 0.034 Uiso 1 1 calc R . .
C32 C 1.4806(2) 1.8225(2) 1.02290(19) 0.0373(5) Uani 1 1 d . . .
H32A H 1.5156 1.7840 1.0767 0.056 Uiso 1 1 calc R . .
H32B H 1.5269 1.9088 1.0499 0.056 Uiso 1 1 calc R . .
H32C H 1.5014 1.7881 0.9517 0.056 Uiso 1 1 calc R . .
N1 N 0.63227(17) 0.88272(16) 0.70809(13) 0.0240(3) Uani 1 1 d . . .
N2 N 0.87354(17) 0.80585(16) 0.70296(14) 0.0258(3) Uani 1 1 d . . .
N3 N 1.01399(17) 1.04756(16) 0.82438(14) 0.0244(3) Uani 1 1 d . . .
N4 N 0.80231(18) 1.09565(16) 0.68689(13) 0.0250(3) Uani 1 1 d . . .
S1 S 0.33630(6) 0.15654(5) 0.67378(5) 0.03279(13) Uani 1 1 d . . .
S2 S 1.29083(7) 1.79783(6) 1.00510(6) 0.03908(14) Uani 1 1 d . . .
Ni1 Ni 0.83072(3) 0.95805(2) 0.72947(2) 0.02245(7) Uani 1 1 d . . .


_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
C1 N1 1.343(2) . ?
C1 C2 1.406(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.370(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.425(3) . ?
C3 H3 0.9300 . ?
C4 N1 1.396(3) . ?
C4 C5 1.398(3) . ?
C5 C6 1.402(3) . ?
C5 C10 1.483(3) . ?
C6 N2 1.384(3) . ?
C6 C7 1.420(3) . ?
C7 C8 1.373(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.399(3) . ?
C8 H8 0.9300 . ?
C9 N2 1.346(2) . ?
C9 H9 0.9300 . ?
C10 C15 1.396(3) . ?
C10 C11 1.401(3) . ?
C11 C12 1.379(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.397(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.396(3) . ?
C13 S1 1.756(2) . ?
C14 C15 1.384(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 S1 1.788(2) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N3 1.346(2) . ?
C17 C18 1.405(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.365(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.423(3) . ?
C19 H19 0.9300 . ?
C20 N3 1.398(3) . ?
C20 C21 1.400(3) . ?
C21 C22 1.403(3) . ?
C21 C26 1.479(3) . ?
C22 N4 1.388(3) . ?
C22 C23 1.418(3) . ?
C23 C24 1.367(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.401(3) . ?
C24 H24 0.9300 . ?
C25 N4 1.346(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.395(3) . ?
C26 C31 1.404(3) . ?
C27 C28 1.388(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.397(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.392(3) . ?
C29 S2 1.759(2) . ?
C30 C31 1.377(3) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 S2 1.783(2) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
N1 Ni1 1.8941(16) . ?
N2 Ni1 1.8841(17) . ?
N3 Ni1 1.8921(17) . ?
N4 Ni1 1.8836(17) . ?

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 C1 C2 111.51(19) . . ?
N1 C1 H1 124.2 . . ?
C2 C1 H1 124.2 . . ?
C3 C2 C1 106.43(18) . . ?
C3 C2 H2 126.8 . . ?
C1 C2 H2 126.8 . . ?
C2 C3 C4 107.38(19) . . ?
C2 C3 H3 126.3 . . ?
C4 C3 H3 126.3 . . ?
N1 C4 C5 123.51(17) . . ?
N1 C4 C3 108.27(17) . . ?
C5 C4 C3 128.1(2) . . ?
C4 C5 C6 122.92(19) . . ?
C4 C5 C10 119.11(18) . . ?
C6 C5 C10 117.97(17) . . ?
N2 C6 C5 123.23(18) . . ?
N2 C6 C7 108.66(17) . . ?
C5 C6 C7 127.6(2) . . ?
C8 C7 C6 107.2(2) . . ?
C8 C7 H7 126.4 . . ?
C6 C7 H7 126.4 . . ?
C7 C8 C9 106.34(18) . . ?
C7 C8 H8 126.8 . . ?
C9 C8 H8 126.8 . . ?
N2 C9 C8 111.4(2) . . ?
N2 C9 H9 124.3 . . ?
C8 C9 H9 124.3 . . ?
C15 C10 C11 117.92(19) . . ?
C15 C10 C5 121.97(17) . . ?
C11 C10 C5 120.09(18) . . ?
C12 C11 C10 121.16(19) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 120.35(18) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 119.15(19) . . ?
C14 C13 S1 124.33(16) . . ?
C12 C13 S1 116.52(14) . . ?
C15 C14 C13 120.00(19) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C10 121.42(18) . . ?
C14 C15 H15 119.3 . . ?
C10 C15 H15 119.3 . . ?
S1 C16 H16A 109.5 . . ?
S1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C18 111.2(2) . . ?
N3 C17 H17 124.4 . . ?
C18 C17 H17 124.4 . . ?
C19 C18 C17 106.68(18) . . ?
C19 C18 H18 126.7 . . ?
C17 C18 H18 126.7 . . ?
C18 C19 C20 107.6(2) . . ?
C18 C19 H19 126.2 . . ?
C20 C19 H19 126.2 . . ?
N3 C20 C21 123.15(17) . . ?
N3 C20 C19 108.08(17) . . ?
C21 C20 C19 128.8(2) . . ?
C20 C21 C22 122.24(19) . . ?
C20 C21 C26 119.52(18) . . ?
C22 C21 C26 118.24(17) . . ?
N4 C22 C21 123.33(17) . . ?
N4 C22 C23 108.35(18) . . ?
C21 C22 C23 128.2(2) . . ?
C24 C23 C22 107.5(2) . . ?
C24 C23 H23 126.2 . . ?
C22 C23 H23 126.2 . . ?
C23 C24 C25 106.46(18) . . ?
C23 C24 H24 126.8 . . ?
C25 C24 H24 126.8 . . ?
N4 C25 C24 111.2(2) . . ?
N4 C25 H25 124.4 . . ?
C24 C25 H25 124.4 . . ?
C27 C26 C31 117.7(2) . . ?
C27 C26 C21 122.64(18) . . ?
C31 C26 C21 119.61(18) . . ?
C28 C27 C26 121.24(19) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C27 C28 C29 120.1(2) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C30 C29 C28 119.0(2) . . ?
C30 C29 S2 115.87(16) . . ?
C28 C29 S2 125.09(17) . . ?
C31 C30 C29 120.46(19) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C30 C31 C26 121.33(19) . . ?
C30 C31 H31 119.3 . . ?
C26 C31 H31 119.3 . . ?
S2 C32 H32A 109.5 . . ?
S2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
S2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C1 N1 C4 106.40(17) . . ?
C1 N1 Ni1 122.35(15) . . ?
C4 N1 Ni1 127.26(12) . . ?
C9 N2 C6 106.37(17) . . ?
C9 N2 Ni1 123.06(15) . . ?
C6 N2 Ni1 129.13(13) . . ?
C17 N3 C20 106.45(17) . . ?
C17 N3 Ni1 121.81(15) . . ?
C20 N3 Ni1 126.29(12) . . ?
C25 N4 C22 106.49(17) . . ?
C25 N4 Ni1 122.46(15) . . ?
C22 N4 Ni1 128.01(13) . . ?
C13 S1 C16 104.14(10) . . ?
C29 S2 C32 103.56(11) . . ?
N4 Ni1 N2 152.87(7) . . ?
N4 Ni1 N3 92.10(7) . . ?
N2 Ni1 N3 94.58(7) . . ?
N4 Ni1 N1 95.03(7) . . ?
N2 Ni1 N1 91.65(7) . . ?
N3 Ni1 N1 151.24(7) . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        29.36
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.062
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound2a
_database_code_depnum_ccdc_archive 'CCDC 1040036'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H24 N4 Ni S2'
_chemical_formula_sum            'C32 H24 N4 Ni S2'
_chemical_formula_weight         587.38

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   9.9075(2)
_cell_length_b                   12.3331(3)
_cell_length_c                   12.4360(3)
_cell_angle_alpha                64.1490(10)
_cell_angle_beta                 69.8930(10)
_cell_angle_gamma                79.4820(10)
_cell_volume                     1283.19(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7263
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      29.66

_exptl_crystal_description       platelet
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8945
_exptl_absorpt_correction_T_max  0.9630
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26379
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         29.42
_reflns_number_total             6911
_reflns_number_gt                5553
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0349P)²+0.5995P] 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         6911
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0828
_refine_ls_wR_factor_gt          0.0762
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
C1 C 0.43421(19) 0.48126(17) 1.16030(17) 0.0233(4) Uani 1 1 d . . .
H1 H 0.4438 0.5635 1.1328 0.028 Uiso 1 1 calc R . .
C2 C 0.50663(19) 0.39048(17) 1.24113(17) 0.0246(4) Uani 1 1 d . . .
H2 H 0.5686 0.4018 1.2767 0.030 Uiso 1 1 calc R . .
C3 C 0.46750(19) 0.28319(17) 1.25647(17) 0.0239(4) Uani 1 1 d . . .
H3 H 0.4977 0.2070 1.3053 0.029 Uiso 1 1 calc R . .
C4 C 0.37143(19) 0.30884(16) 1.18383(16) 0.0205(3) Uani 1 1 d . . .
C5 C 0.32838(18) 0.22639(15) 1.15332(16) 0.0196(3) Uani 1 1 d . . .
C6 C 0.26233(19) 0.26288(15) 1.05841(16) 0.0200(3) Uani 1 1 d . . .
C7 C 0.21390(19) 0.19633(16) 1.00923(17) 0.0211(4) Uani 1 1 d . . .
H7 H 0.2216 0.1131 1.0343 0.025 Uiso 1 1 calc R . .
C8 C 0.15382(19) 0.27818(16) 0.91809(17) 0.0216(4) Uani 1 1 d . . .
H8 H 0.1140 0.2610 0.8698 0.026 Uiso 1 1 calc R . .
C9 C 0.16487(18) 0.39380(16) 0.91263(16) 0.0197(3) Uani 1 1 d . . .
C10 C 0.35752(18) 0.09599(15) 1.22168(16) 0.0201(3) Uani 1 1 d . . .
C11 C 0.4293(2) 0.02266(16) 1.15795(17) 0.0231(4) Uani 1 1 d . . .
H11 H 0.4636 0.0571 1.0710 0.028 Uiso 1 1 calc R . .
C12 C 0.4502(2) -0.10027(16) 1.22172(17) 0.0237(4) Uani 1 1 d . . .
H12 H 0.4979 -0.1474 1.1775 0.028 Uiso 1 1 calc R . .
C13 C 0.40003(19) -0.15321(16) 1.35170(17) 0.0208(3) Uani 1 1 d . . .
C14 C 0.33376(19) -0.07994(16) 1.41655(17) 0.0231(4) Uani 1 1 d . . .
H14 H 0.3042 -0.1139 1.5036 0.028 Uiso 1 1 calc R . .
C15 C 0.31170(19) 0.04219(16) 1.35296(17) 0.0228(4) Uani 1 1 d . . .
H15 H 0.2660 0.0894 1.3976 0.027 Uiso 1 1 calc R . .
C16 C 0.5023(3) -0.36924(19) 1.3274(2) 0.0422(6) Uani 1 1 d . . .
H16A H 0.4456 -0.3507 1.2721 0.063 Uiso 1 1 calc R . .
H16B H 0.5149 -0.4551 1.3682 0.063 Uiso 1 1 calc R . .
H16C H 0.5946 -0.3342 1.2800 0.063 Uiso 1 1 calc R . .
C17 C 0.2009(2) 0.68321(17) 1.13932(18) 0.0262(4) Uani 1 1 d . . .
H17 H 0.2082 0.6208 1.2142 0.031 Uiso 1 1 calc R . .
C18 C 0.1783(2) 0.80520(18) 1.11974(19) 0.0317(4) Uani 1 1 d . . .
H18 H 0.1694 0.8373 1.1771 0.038 Uiso 1 1 calc R . .
C19 C 0.1719(2) 0.86782(17) 0.99923(19) 0.0274(4) Uani 1 1 d . . .
H19 H 0.1587 0.9509 0.9593 0.033 Uiso 1 1 calc R . .
C20 C 0.18942(19) 0.78179(16) 0.94639(18) 0.0222(4) Uani 1 1 d . . .
C21 C 0.15718(18) 0.80339(16) 0.83617(17) 0.0207(3) Uani 1 1 d . . .
C22 C 0.13104(19) 0.70853(16) 0.81297(16) 0.0201(3) Uani 1 1 d . . .
C23 C 0.0871(2) 0.70626(16) 0.71560(17) 0.0232(4) Uani 1 1 d . . .
H23 H 0.0659 0.7731 0.6495 0.028 Uiso 1 1 calc R . .
C24 C 0.0821(2) 0.58744(16) 0.73749(17) 0.0237(4) Uani 1 1 d . . .
H24 H 0.0553 0.5587 0.6902 0.028 Uiso 1 1 calc R . .
C25 C 0.12576(18) 0.51738(16) 0.84610(16) 0.0194(3) Uani 1 1 d . . .
C26 C 0.14473(19) 0.93034(16) 0.74806(17) 0.0213(4) Uani 1 1 d . . .
C27 C 0.2500(2) 1.01140(16) 0.71177(18) 0.0249(4) Uani 1 1 d . . .
H27 H 0.3318 0.9832 0.7381 0.030 Uiso 1 1 calc R . .
C28 C 0.2354(2) 1.13278(16) 0.63753(18) 0.0256(4) Uani 1 1 d . . .
H28 H 0.3075 1.1847 0.6140 0.031 Uiso 1 1 calc R . .
C29 C 0.1134(2) 1.17719(16) 0.59808(17) 0.0252(4) Uani 1 1 d . . .
C30 C 0.0104(2) 1.09659(17) 0.62895(18) 0.0260(4) Uani 1 1 d . . .
H30 H -0.0694 1.1245 0.5996 0.031 Uiso 1 1 calc R . .
C31 C 0.02571(19) 0.97530(17) 0.70294(17) 0.0232(4) Uani 1 1 d . . .
H31 H -0.0443 0.9229 0.7229 0.028 Uiso 1 1 calc R . .
C32 C 0.2100(2) 1.40678(18) 0.5171(2) 0.0386(5) Uani 1 1 d . . .
H32A H 0.2020 1.3862 0.6029 0.058 Uiso 1 1 calc R . .
H32B H 0.1947 1.4923 0.4757 0.058 Uiso 1 1 calc R . .
H32C H 0.3043 1.3831 0.4761 0.058 Uiso 1 1 calc R . .
N1 N 0.35022(16) 0.43432(13) 1.12828(14) 0.0204(3) Uani 1 1 d . . .
N2 N 0.23090(16) 0.38253(13) 0.99600(14) 0.0193(3) Uani 1 1 d . . .
N3 N 0.15123(15) 0.59085(13) 0.89156(13) 0.0192(3) Uani 1 1 d . . .
N4 N 0.21079(16) 0.66777(13) 1.03627(14) 0.0218(3) Uani 1 1 d . . .
S1 S 0.41261(6) -0.30914(4) 1.44228(5) 0.03062(12) Uani 1 1 d . . .
S2 S 0.07828(7) 1.33018(5) 0.51106(6) 0.04392(16) Uani 1 1 d . . .
Ni1 Ni 0.23850(2) 0.52059(2) 1.01768(2) 0.01880(7) Uani 1 1 d . . .


_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
C1 N1 1.338(2) . ?
C1 C2 1.414(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.362(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.433(2) . ?
C3 H3 0.9300 . ?
C4 N1 1.402(2) . ?
C4 C5 1.402(2) . ?
C5 C6 1.409(2) . ?
C5 C10 1.483(2) . ?
C6 N2 1.370(2) . ?
C6 C7 1.436(2) . ?
C7 C8 1.380(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.420(2) . ?
C8 H8 0.9300 . ?
C9 N2 1.353(2) . ?
C9 C25 1.436(2) . ?
C10 C11 1.398(2) . ?
C10 C15 1.403(2) . ?
C11 C12 1.386(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.390(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.398(2) . ?
C13 S1 1.7614(18) . ?
C14 C15 1.379(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 S1 1.786(2) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N4 1.345(2) . ?
C17 C18 1.403(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.373(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.432(2) . ?
C19 H19 0.9300 . ?
C20 N4 1.398(2) . ?
C20 C21 1.415(2) . ?
C21 C22 1.405(2) . ?
C21 C26 1.481(2) . ?
C22 N3 1.376(2) . ?
C22 C23 1.433(2) . ?
C23 C24 1.376(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.416(2) . ?
C24 H24 0.9300 . ?
C25 N3 1.354(2) . ?
C26 C27 1.398(3) . ?
C26 C31 1.399(2) . ?
C27 C28 1.386(2) . ?
C27 H27 0.9300 . ?
C28 C29 1.391(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.395(3) . ?
C29 S2 1.7581(19) . ?
C30 C31 1.386(3) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 S2 1.784(2) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
N1 Ni1 1.8946(14) . ?
N2 Ni1 1.8544(14) . ?
N3 Ni1 1.8527(14) . ?
N4 Ni1 1.8879(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 111.70(16) . . ?
N1 C1 H1 124.1 . . ?
C2 C1 H1 124.1 . . ?
C3 C2 C1 106.32(16) . . ?
C3 C2 H2 126.8 . . ?
C1 C2 H2 126.8 . . ?
C2 C3 C4 107.63(16) . . ?
C2 C3 H3 126.2 . . ?
C4 C3 H3 126.2 . . ?
N1 C4 C5 124.89(15) . . ?
N1 C4 C3 107.94(15) . . ?
C5 C4 C3 126.10(16) . . ?
C4 C5 C6 122.57(16) . . ?
C4 C5 C10 118.37(15) . . ?
C6 C5 C10 119.04(15) . . ?
N2 C6 C5 120.22(15) . . ?
N2 C6 C7 107.52(15) . . ?
C5 C6 C7 132.25(16) . . ?
C8 C7 C6 107.61(15) . . ?
C8 C7 H7 126.2 . . ?
C6 C7 H7 126.2 . . ?
C7 C8 C9 106.39(15) . . ?
C7 C8 H8 126.8 . . ?
C9 C8 H8 126.8 . . ?
N2 C9 C8 109.55(15) . . ?
N2 C9 C25 111.64(14) . . ?
C8 C9 C25 138.81(16) . . ?
C11 C10 C15 117.97(16) . . ?
C11 C10 C5 121.37(16) . . ?
C15 C10 C5 120.65(15) . . ?
C12 C11 C10 121.34(17) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C13 120.13(16) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C14 118.97(16) . . ?
C12 C13 S1 124.16(13) . . ?
C14 C13 S1 116.86(14) . . ?
C15 C14 C13 120.78(17) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C10 120.70(16) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
S1 C16 H16A 109.5 . . ?
S1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 111.51(17) . . ?
N4 C17 H17 124.2 . . ?
C18 C17 H17 124.2 . . ?
C19 C18 C17 106.52(16) . . ?
C19 C18 H18 126.7 . . ?
C17 C18 H18 126.7 . . ?
C18 C19 C20 107.41(16) . . ?
C18 C19 H19 126.3 . . ?
C20 C19 H19 126.3 . . ?
N4 C20 C21 124.98(15) . . ?
N4 C20 C19 107.83(15) . . ?
C21 C20 C19 125.65(17) . . ?
C22 C21 C20 121.57(16) . . ?
C22 C21 C26 120.60(16) . . ?
C20 C21 C26 117.77(15) . . ?
N3 C22 C21 120.02(15) . . ?
N3 C22 C23 107.43(15) . . ?
C21 C22 C23 132.53(17) . . ?
C24 C23 C22 107.73(16) . . ?
C24 C23 H23 126.1 . . ?
C22 C23 H23 126.1 . . ?
C23 C24 C25 106.58(15) . . ?
C23 C24 H24 126.7 . . ?
C25 C24 H24 126.7 . . ?
N3 C25 C24 109.61(15) . . ?
N3 C25 C9 111.84(15) . . ?
C24 C25 C9 138.11(16) . . ?
C27 C26 C31 117.53(17) . . ?
C27 C26 C21 120.38(16) . . ?
C31 C26 C21 122.02(16) . . ?
C28 C27 C26 121.59(17) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C27 C28 C29 120.21(18) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C28 C29 C30 118.84(17) . . ?
C28 C29 S2 124.37(15) . . ?
C30 C29 S2 116.79(14) . . ?
C31 C30 C29 120.60(17) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C26 121.10(17) . . ?
C30 C31 H31 119.4 . . ?
C26 C31 H31 119.4 . . ?
S2 C32 H32A 109.5 . . ?
S2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
S2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C1 N1 C4 106.31(14) . . ?
C1 N1 Ni1 126.71(13) . . ?
C4 N1 Ni1 126.76(11) . . ?
C9 N2 C6 108.92(14) . . ?
C9 N2 Ni1 116.89(12) . . ?
C6 N2 Ni1 133.60(12) . . ?
C25 N3 C22 108.59(14) . . ?
C25 N3 Ni1 116.86(12) . . ?
C22 N3 Ni1 133.02(12) . . ?
C17 N4 C20 106.67(14) . . ?
C17 N4 Ni1 127.11(13) . . ?
C20 N4 Ni1 126.15(12) . . ?
C13 S1 C16 103.13(10) . . ?
C29 S2 C32 103.98(10) . . ?
N3 Ni1 N2 82.43(6) . . ?
N3 Ni1 N4 89.30(6) . . ?
N2 Ni1 N4 169.09(6) . . ?
N3 Ni1 N1 169.53(6) . . ?
N2 Ni1 N1 90.10(6) . . ?
N4 Ni1 N1 98.97(6) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        29.42
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.063
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound3a
_database_code_depnum_ccdc_archive 'CCDC 1040037'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H26 N4 S2, C H Cl3'
_chemical_formula_sum            'C33 H27 Cl3 N4 S2'
_chemical_formula_weight         650.06

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'
S S 0.1246 0.1234 '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           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   8.9232(2)
_cell_length_b                   12.3869(3)
_cell_length_c                   14.6782(4)
_cell_angle_alpha                75.7490(10)
_cell_angle_beta                 75.0970(10)
_cell_angle_gamma                86.5210(10)
_cell_volume                     1519.57(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7203
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      29.62

_exptl_crystal_description       platelet
_exptl_crystal_colour            dark-blue
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9501
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30752
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         29.48
_reflns_number_total             8155
_reflns_number_gt                5472
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0593P)²+0.9554P] 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         8155
_refine_ls_number_parameters     381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1213
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
C1 C 0.8494(3) 0.4147(2) 0.26152(18) 0.0348(6) Uani 1 1 d . . .
H1A H 0.7856 0.3648 0.2510 0.042 Uiso 1 1 calc R . .
C2 C 0.9543(3) 0.3863(2) 0.31884(18) 0.0349(6) Uani 1 1 d . . .
H2 H 0.9736 0.3151 0.3527 0.042 Uiso 1 1 calc R . .
C3 C 1.0246(3) 0.4839(2) 0.31621(17) 0.0314(5) Uani 1 1 d . . .
H3A H 1.0996 0.4905 0.3483 0.038 Uiso 1 1 calc R . .
C4 C 0.9616(2) 0.57109(19) 0.25598(16) 0.0258(5) Uani 1 1 d . . .
C5 C 0.9961(2) 0.68634(18) 0.22827(15) 0.0236(4) Uani 1 1 d . . .
C6 C 0.9275(2) 0.76359(19) 0.16533(16) 0.0242(4) Uani 1 1 d . . .
C7 C 0.9478(3) 0.88248(19) 0.13881(17) 0.0286(5) Uani 1 1 d . . .
H7 H 1.0124 0.9227 0.1591 0.034 Uiso 1 1 calc R . .
C8 C 0.8547(3) 0.9249(2) 0.07846(17) 0.0285(5) Uani 1 1 d . . .
H8 H 0.8433 0.9996 0.0495 0.034 Uiso 1 1 calc R . .
C9 C 0.7776(2) 0.83204(19) 0.06820(15) 0.0237(4) Uani 1 1 d . . .
C10 C 1.1100(2) 0.72567(18) 0.27190(15) 0.0231(4) Uani 1 1 d . . .
C11 C 1.0729(3) 0.7231(2) 0.37030(18) 0.0391(6) Uani 1 1 d . . .
H11 H 0.9759 0.6973 0.4090 0.047 Uiso 1 1 calc R . .
C12 C 1.1778(3) 0.7583(2) 0.41135(17) 0.0391(6) Uani 1 1 d . . .
H12 H 1.1500 0.7568 0.4772 0.047 Uiso 1 1 calc R . .
C13 C 1.3239(2) 0.79593(18) 0.35606(16) 0.0251(5) Uani 1 1 d . . .
C14 C 1.3631(2) 0.7989(2) 0.25691(16) 0.0277(5) Uani 1 1 d . . .
H14 H 1.4606 0.8237 0.2185 0.033 Uiso 1 1 calc R . .
C15 C 1.2557(3) 0.76469(19) 0.21604(16) 0.0273(5) Uani 1 1 d . . .
H15 H 1.2819 0.7680 0.1499 0.033 Uiso 1 1 calc R . .
C16 C 1.6343(3) 0.8441(3) 0.3356(2) 0.0421(6) Uani 1 1 d . . .
H16A H 1.6572 0.7738 0.3186 0.063 Uiso 1 1 calc R . .
H16B H 1.7109 0.8602 0.3659 0.063 Uiso 1 1 calc R . .
H16C H 1.6356 0.9016 0.2780 0.063 Uiso 1 1 calc R . .
C17 C 0.6689(2) 0.84013(18) 0.00885(15) 0.0239(4) Uani 1 1 d . . .
C18 C 0.6408(3) 0.93345(19) -0.06126(17) 0.0280(5) Uani 1 1 d . . .
H18 H 0.6898 1.0023 -0.0789 0.034 Uiso 1 1 calc R . .
C19 C 0.5269(3) 0.90430(19) -0.09921(16) 0.0270(5) Uani 1 1 d . . .
H19 H 0.4860 0.9497 -0.1475 0.032 Uiso 1 1 calc R . .
C20 C 0.4841(2) 0.79297(18) -0.05130(15) 0.0228(4) Uani 1 1 d . . .
C21 C 0.3645(2) 0.72788(18) -0.06040(15) 0.0221(4) Uani 1 1 d . . .
C22 C 0.3197(2) 0.62306(18) -0.00135(15) 0.0234(4) Uani 1 1 d . . .
C23 C 0.2081(3) 0.54757(19) -0.00695(16) 0.0276(5) Uani 1 1 d . . .
H23 H 0.1465 0.5605 -0.0509 0.033 Uiso 1 1 calc R . .
C24 C 0.2099(3) 0.4539(2) 0.06402(17) 0.0318(5) Uani 1 1 d . . .
H24 H 0.1499 0.3902 0.0783 0.038 Uiso 1 1 calc R . .
C25 C 0.3220(3) 0.4727(2) 0.11240(17) 0.0311(5) Uani 1 1 d . . .
H25 H 0.3459 0.4210 0.1644 0.037 Uiso 1 1 calc R . .
C26 C 0.2843(2) 0.77900(17) -0.13785(15) 0.0217(4) Uani 1 1 d . . .
C27 C 0.1235(2) 0.79225(18) -0.11662(15) 0.0242(4) Uani 1 1 d . . .
H27 H 0.0654 0.7677 -0.0529 0.029 Uiso 1 1 calc R . .
C28 C 0.0484(3) 0.84137(18) -0.18857(16) 0.0257(5) Uani 1 1 d . . .
H28 H -0.0587 0.8499 -0.1728 0.031 Uiso 1 1 calc R . .
C29 C 0.1343(3) 0.87788(18) -0.28462(16) 0.0264(5) Uani 1 1 d . . .
C30 C 0.2952(3) 0.8646(2) -0.30686(16) 0.0297(5) Uani 1 1 d . . .
H30 H 0.3533 0.8881 -0.3707 0.036 Uiso 1 1 calc R . .
C31 C 0.3683(3) 0.81657(19) -0.23418(15) 0.0266(5) Uani 1 1 d . . .
H31 H 0.4756 0.8092 -0.2498 0.032 Uiso 1 1 calc R . .
C32 C -0.1516(3) 0.9333(3) -0.3292(2) 0.0495(7) Uani 1 1 d . . .
H32A H -0.1807 0.8574 -0.2971 0.074 Uiso 1 1 calc R . .
H32B H -0.2059 0.9598 -0.3790 0.074 Uiso 1 1 calc R . .
H32C H -0.1779 0.9785 -0.2828 0.074 Uiso 1 1 calc R . .
N1 N 0.8542(2) 0.52484(16) 0.22372(14) 0.0299(4) Uani 1 1 d . . .
H1 H 0.7995 0.5608 0.1857 0.036 Uiso 1 1 calc R . .
N2 N 0.8199(2) 0.73611(15) 0.11989(13) 0.0242(4) Uani 1 1 d . . .
N3 N 0.5747(2) 0.75639(15) 0.01369(13) 0.0231(4) Uani 1 1 d . . .
H3 H 0.5715 0.6908 0.0513 0.028 Uiso 1 1 calc R . .
N4 N 0.3880(2) 0.57150(16) 0.07507(13) 0.0272(4) Uani 1 1 d . . .
S1 S 1.44683(7) 0.83795(6) 0.41793(5) 0.03690(17) Uani 1 1 d . . .
S2 S 0.05388(8) 0.94100(6) -0.38281(5) 0.03989(17) Uani 1 1 d . . .
C33 C 0.5891(3) 0.5974(2) 0.57592(19) 0.0417(6) Uani 1 1 d . . .
H33 H 0.4914 0.6239 0.5596 0.050 Uiso 1 1 calc R . .
Cl1 Cl 0.68656(9) 0.71108(6) 0.58867(5) 0.04968(19) Uani 1 1 d . . .
Cl2 Cl 0.70439(9) 0.54299(7) 0.48166(6) 0.0582(2) Uani 1 1 d . . .
Cl3 Cl 0.54852(9) 0.49324(8) 0.68411(6) 0.0629(2) Uani 1 1 d . . .


_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
C1 N1 1.340(3) . ?
C1 C2 1.388(3) . ?
C1 H1A 0.9300 . ?
C2 C3 1.383(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.406(3) . ?
C3 H3A 0.9300 . ?
C4 N1 1.380(3) . ?
C4 C5 1.415(3) . ?
C5 C6 1.389(3) . ?
C5 C10 1.492(3) . ?
C6 N2 1.401(3) . ?
C6 C7 1.438(3) . ?
C7 C8 1.359(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.433(3) . ?
C8 H8 0.9300 . ?
C9 N2 1.334(3) . ?
C9 C17 1.445(3) . ?
C10 C11 1.389(3) . ?
C10 C15 1.389(3) . ?
C11 C12 1.378(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.385(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.398(3) . ?
C13 S1 1.764(2) . ?
C14 C15 1.388(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 S1 1.788(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N3 1.352(3) . ?
C17 C18 1.404(3) . ?
C18 C19 1.381(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.411(3) . ?
C19 H19 0.9300 . ?
C20 N3 1.381(3) . ?
C20 C21 1.427(3) . ?
C21 C22 1.388(3) . ?
C21 C26 1.488(3) . ?
C22 N4 1.410(3) . ?
C22 C23 1.437(3) . ?
C23 C24 1.358(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.426(3) . ?
C24 H24 0.9300 . ?
C25 N4 1.318(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.396(3) . ?
C26 C31 1.397(3) . ?
C27 C28 1.390(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.397(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.397(3) . ?
C29 S2 1.764(2) . ?
C30 C31 1.384(3) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 S2 1.798(3) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
N1 H1 0.8600 . ?
N3 H3 0.8600 . ?
C33 Cl2 1.752(3) . ?
C33 Cl3 1.752(3) . ?
C33 Cl1 1.771(3) . ?
C33 H33 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
N1 C1 C2 109.6(2) . . ?
N1 C1 H1A 125.2 . . ?
C2 C1 H1A 125.2 . . ?
C3 C2 C1 107.1(2) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
C2 C3 C4 107.3(2) . . ?
C2 C3 H3A 126.4 . . ?
C4 C3 H3A 126.4 . . ?
N1 C4 C3 107.4(2) . . ?
N1 C4 C5 122.9(2) . . ?
C3 C4 C5 129.7(2) . . ?
C6 C5 C4 123.65(19) . . ?
C6 C5 C10 119.12(19) . . ?
C4 C5 C10 117.21(19) . . ?
C5 C6 N2 124.01(19) . . ?
C5 C6 C7 127.13(19) . . ?
N2 C6 C7 108.81(19) . . ?
C8 C7 C6 106.96(19) . . ?
C8 C7 H7 126.5 . . ?
C6 C7 H7 126.5 . . ?
C7 C8 C9 106.6(2) . . ?
C7 C8 H8 126.7 . . ?
C9 C8 H8 126.7 . . ?
N2 C9 C8 111.35(18) . . ?
N2 C9 C17 123.87(19) . . ?
C8 C9 C17 124.8(2) . . ?
C11 C10 C15 118.18(19) . . ?
C11 C10 C5 120.51(19) . . ?
C15 C10 C5 121.31(19) . . ?
C12 C11 C10 120.9(2) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 121.0(2) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 118.7(2) . . ?
C12 C13 S1 116.31(17) . . ?
C14 C13 S1 124.94(17) . . ?
C15 C14 C13 119.7(2) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C10 121.4(2) . . ?
C14 C15 H15 119.3 . . ?
C10 C15 H15 119.3 . . ?
S1 C16 H16A 109.5 . . ?
S1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C18 108.52(18) . . ?
N3 C17 C9 124.3(2) . . ?
C18 C17 C9 127.2(2) . . ?
C19 C18 C17 107.5(2) . . ?
C19 C18 H18 126.2 . . ?
C17 C18 H18 126.2 . . ?
C18 C19 C20 107.47(19) . . ?
C18 C19 H19 126.3 . . ?
C20 C19 H19 126.3 . . ?
N3 C20 C19 107.33(18) . . ?
N3 C20 C21 123.9(2) . . ?
C19 C20 C21 128.70(19) . . ?
C22 C21 C20 123.98(19) . . ?
C22 C21 C26 119.74(18) . . ?
C20 C21 C26 116.28(19) . . ?
C21 C22 N4 122.48(19) . . ?
C21 C22 C23 128.97(19) . . ?
N4 C22 C23 108.49(19) . . ?
C24 C23 C22 107.0(2) . . ?
C24 C23 H23 126.5 . . ?
C22 C23 H23 126.5 . . ?
C23 C24 C25 106.3(2) . . ?
C23 C24 H24 126.9 . . ?
C25 C24 H24 126.9 . . ?
N4 C25 C24 112.4(2) . . ?
N4 C25 H25 123.8 . . ?
C24 C25 H25 123.8 . . ?
C27 C26 C31 117.89(19) . . ?
C27 C26 C21 121.29(19) . . ?
C31 C26 C21 120.82(19) . . ?
C28 C27 C26 121.4(2) . . ?
C28 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C27 C28 C29 119.9(2) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C28 119.2(2) . . ?
C30 C29 S2 116.24(17) . . ?
C28 C29 S2 124.51(17) . . ?
C31 C30 C29 120.2(2) . . ?
C31 C30 H30 119.9 . . ?
C29 C30 H30 119.9 . . ?
C30 C31 C26 121.4(2) . . ?
C30 C31 H31 119.3 . . ?
C26 C31 H31 119.3 . . ?
S2 C32 H32A 109.5 . . ?
S2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
S2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C1 N1 C4 108.6(2) . . ?
C1 N1 H1 125.7 . . ?
C4 N1 H1 125.7 . . ?
C9 N2 C6 106.26(18) . . ?
C17 N3 C20 109.16(18) . . ?
C17 N3 H3 125.4 . . ?
C20 N3 H3 125.4 . . ?
C25 N4 C22 105.86(19) . . ?
C13 S1 C16 103.69(11) . . ?
C29 S2 C32 103.56(12) . . ?
Cl2 C33 Cl3 109.81(16) . . ?
Cl2 C33 Cl1 109.44(15) . . ?
Cl3 C33 Cl1 110.87(15) . . ?
Cl2 C33 H33 108.9 . . ?
Cl3 C33 H33 108.9 . . ?
Cl1 C33 H33 108.9 . . ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        29.48
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.066
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound4a
_database_code_depnum_ccdc_archive 'CCDC 1040038'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H48 N8 S4 Zn2'
_chemical_formula_sum            'C64 H48 N8 S4 Zn2'
_chemical_formula_weight         1188.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2840 1.4300 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

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

_cell_length_a                   15.1355(4)
_cell_length_b                   14.9332(4)
_cell_length_c                   24.9048(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.3990(10)
_cell_angle_gamma                90.00
_cell_volume                     5400.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7660
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      29.72

_exptl_crystal_description       platelet
_exptl_crystal_colour            dark-purple
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2447
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9176
_exptl_absorpt_correction_T_max  0.9575
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            62112
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         30.09
_reflns_number_total             15675
_reflns_number_gt                9677
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0773P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15675
_refine_ls_number_parameters     707
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1580
_refine_ls_wR_factor_gt          0.1310
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
C1 C 0.1159(2) 0.4985(2) 0.05227(14) 0.0334(7) Uani 1 1 d . . .
H1 H 0.1581 0.4696 0.0374 0.040 Uiso 1 1 calc R . .
C2 C 0.0758(2) 0.4607(2) 0.09165(15) 0.0395(8) Uani 1 1 d . . .
H2 H 0.0867 0.4035 0.1069 0.047 Uiso 1 1 calc R . .
C3 C 0.0185(2) 0.5228(2) 0.10337(13) 0.0325(7) Uani 1 1 d . . .
H3 H -0.0170 0.5163 0.1282 0.039 Uiso 1 1 calc R . .
C4 C 0.0229(2) 0.5997(2) 0.07051(12) 0.0267(6) Uani 1 1 d . . .
C5 C -0.0240(2) 0.6806(2) 0.06857(12) 0.0251(6) Uani 1 1 d . . .
C6 C -0.0097(2) 0.7580(2) 0.03998(13) 0.0269(6) Uani 1 1 d . . .
C7 C -0.0709(2) 0.8326(2) 0.02548(15) 0.0342(8) Uani 1 1 d . . .
H7 H -0.1254 0.8405 0.0351 0.041 Uiso 1 1 calc R . .
C8 C -0.0340(2) 0.8908(2) -0.00552(15) 0.0348(8) Uani 1 1 d . . .
H8 H -0.0598 0.9441 -0.0220 0.042 Uiso 1 1 calc R . .
C9 C 0.0513(2) 0.8526(2) -0.00706(13) 0.0268(6) Uani 1 1 d . . .
C10 C -0.0964(2) 0.6854(2) 0.09832(13) 0.0257(6) Uani 1 1 d . . .
C11 C -0.1686(2) 0.6237(2) 0.08807(13) 0.0275(7) Uani 1 1 d . . .
H11 H -0.1699 0.5757 0.0641 0.033 Uiso 1 1 calc R . .
C12 C -0.2380(2) 0.6337(2) 0.11349(13) 0.0303(7) Uani 1 1 d . . .
H12 H -0.2876 0.5943 0.1047 0.036 Uiso 1 1 calc R . .
C13 C -0.2353(2) 0.7014(2) 0.15187(12) 0.0278(7) Uani 1 1 d . . .
C14 C -0.1619(2) 0.7601(2) 0.16423(14) 0.0373(8) Uani 1 1 d . . .
H14 H -0.1579 0.8044 0.1910 0.045 Uiso 1 1 calc R . .
C15 C -0.0942(2) 0.7535(2) 0.13709(14) 0.0356(8) Uani 1 1 d . . .
H15 H -0.0465 0.7951 0.1447 0.043 Uiso 1 1 calc R . .
C16 C -0.3384(3) 0.8279(3) 0.18772(18) 0.0553(11) Uani 1 1 d . . .
H16A H -0.2852 0.8532 0.2140 0.083 Uiso 1 1 calc R . .
H16B H -0.3922 0.8412 0.1994 0.083 Uiso 1 1 calc R . .
H16C H -0.3451 0.8532 0.1514 0.083 Uiso 1 1 calc R . .
C17 C 0.1192(2) 0.8896(2) -0.03151(13) 0.0264(6) Uani 1 1 d . . .
C18 C 0.1060(2) 0.9508(2) -0.07650(13) 0.0315(7) Uani 1 1 d . . .
H18 H 0.0516 0.9801 -0.0949 0.038 Uiso 1 1 calc R . .
C19 C 0.1892(2) 0.9581(2) -0.08751(14) 0.0319(7) Uani 1 1 d . . .
H19 H 0.2017 0.9933 -0.1153 0.038 Uiso 1 1 calc R . .
C20 C 0.2532(2) 0.9027(2) -0.04920(12) 0.0249(6) Uani 1 1 d . . .
C21 C 0.3469(2) 0.88901(19) -0.04591(12) 0.0233(6) Uani 1 1 d . . .
C22 C 0.4115(2) 0.8474(2) -0.00232(12) 0.0251(6) Uani 1 1 d . . .
C23 C 0.5016(2) 0.8189(2) -0.00152(13) 0.0329(8) Uani 1 1 d . . .
H23 H 0.5299 0.8275 -0.0298 0.039 Uiso 1 1 calc R . .
C24 C 0.5388(2) 0.7768(3) 0.04802(14) 0.0410(9) Uani 1 1 d . . .
H24 H 0.5972 0.7514 0.0602 0.049 Uiso 1 1 calc R . .
C25 C 0.4717(2) 0.7792(3) 0.07725(14) 0.0390(8) Uani 1 1 d . . .
H25 H 0.4791 0.7541 0.1124 0.047 Uiso 1 1 calc R . .
C26 C 0.3767(2) 0.9165(2) -0.09582(12) 0.0235(6) Uani 1 1 d . . .
C27 C 0.3297(2) 0.8824(2) -0.14855(12) 0.0267(6) Uani 1 1 d . . .
H27 H 0.2781 0.8464 -0.1524 0.032 Uiso 1 1 calc R . .
C28 C 0.3592(2) 0.9017(2) -0.19505(12) 0.0287(7) Uani 1 1 d . . .
H28 H 0.3281 0.8775 -0.2296 0.034 Uiso 1 1 calc R . .
C29 C 0.4350(2) 0.9569(2) -0.19058(12) 0.0256(6) Uani 1 1 d . . .
C30 C 0.4823(2) 0.9908(2) -0.13811(13) 0.0280(7) Uani 1 1 d . . .
H30 H 0.5335 1.0274 -0.1343 0.034 Uiso 1 1 calc R . .
C31 C 0.4532(2) 0.9700(2) -0.09166(13) 0.0279(7) Uani 1 1 d . . .
H31 H 0.4856 0.9925 -0.0569 0.033 Uiso 1 1 calc R . .
C32 C 0.5637(3) 1.0468(3) -0.23215(16) 0.0503(10) Uani 1 1 d . . .
H32A H 0.5508 1.0997 -0.2138 0.075 Uiso 1 1 calc R . .
H32B H 0.5828 1.0635 -0.2644 0.075 Uiso 1 1 calc R . .
H32C H 0.6119 1.0134 -0.2068 0.075 Uiso 1 1 calc R . .
C33 C 0.0353(2) 0.7227(2) -0.12353(14) 0.0333(7) Uani 1 1 d . . .
H33 H -0.0173 0.7412 -0.1144 0.040 Uiso 1 1 calc R . .
C34 C 0.0483(3) 0.7320(2) -0.17649(14) 0.0374(8) Uani 1 1 d . . .
H34 H 0.0069 0.7562 -0.2081 0.045 Uiso 1 1 calc R . .
C35 C 0.1346(3) 0.6980(2) -0.17258(13) 0.0342(8) Uani 1 1 d . . .
H35 H 0.1629 0.6954 -0.2012 0.041 Uiso 1 1 calc R . .
C36 C 0.1721(2) 0.6676(2) -0.11664(12) 0.0256(6) Uani 1 1 d . . .
C37 C 0.2587(2) 0.6302(2) -0.09378(12) 0.0251(6) Uani 1 1 d . . .
C38 C 0.2995(2) 0.6103(2) -0.03657(12) 0.0258(6) Uani 1 1 d . . .
C39 C 0.3791(2) 0.5571(2) -0.01266(13) 0.0321(7) Uani 1 1 d . . .
H39 H 0.4163 0.5301 -0.0319 0.039 Uiso 1 1 calc R . .
C40 C 0.3908(2) 0.5531(2) 0.04414(13) 0.0333(7) Uani 1 1 d . . .
H40 H 0.4362 0.5218 0.0704 0.040 Uiso 1 1 calc R . .
C41 C 0.3199(2) 0.6061(2) 0.05442(12) 0.0280(7) Uani 1 1 d . . .
C42 C 0.3162(2) 0.6104(2) -0.13206(12) 0.0269(7) Uani 1 1 d . . .
C43 C 0.2849(2) 0.5545(2) -0.17839(13) 0.0312(7) Uani 1 1 d . . .
H43 H 0.2267 0.5288 -0.1854 0.037 Uiso 1 1 calc R . .
C44 C 0.3370(2) 0.5364(2) -0.21365(13) 0.0309(7) Uani 1 1 d . . .
H44 H 0.3148 0.4977 -0.2437 0.037 Uiso 1 1 calc R . .
C45 C 0.4233(2) 0.5759(2) -0.20476(13) 0.0310(7) Uani 1 1 d . . .
C46 C 0.4558(2) 0.6317(2) -0.15952(14) 0.0372(8) Uani 1 1 d . . .
H46 H 0.5135 0.6581 -0.1532 0.045 Uiso 1 1 calc R . .
C47 C 0.4029(2) 0.6490(2) -0.12312(14) 0.0338(8) Uani 1 1 d . . .
H47 H 0.4256 0.6867 -0.0926 0.041 Uiso 1 1 calc R . .
C48 C 0.4715(3) 0.4451(3) -0.26976(16) 0.0536(11) Uani 1 1 d . . .
H48A H 0.4828 0.4092 -0.2366 0.080 Uiso 1 1 calc R . .
H48B H 0.5115 0.4264 -0.2914 0.080 Uiso 1 1 calc R . .
H48C H 0.4085 0.4381 -0.2916 0.080 Uiso 1 1 calc R . .
C49 C 0.3054(2) 0.6328(2) 0.10691(12) 0.0276(7) Uani 1 1 d . . .
C50 C 0.3178(3) 0.5830(2) 0.15682(13) 0.0378(8) Uani 1 1 d . . .
H50 H 0.3416 0.5254 0.1639 0.045 Uiso 1 1 calc R . .
C51 C 0.2879(2) 0.6367(2) 0.19248(13) 0.0357(8) Uani 1 1 d . . .
H51 H 0.2872 0.6218 0.2286 0.043 Uiso 1 1 calc R . .
C52 C 0.2579(2) 0.7193(2) 0.16480(12) 0.0271(7) Uani 1 1 d . . .
C53 C 0.2268(2) 0.7955(2) 0.18726(12) 0.0246(6) Uani 1 1 d . . .
C54 C 0.2152(2) 0.8814(2) 0.16375(12) 0.0259(6) Uani 1 1 d . . .
C55 C 0.1796(2) 0.9590(2) 0.18376(14) 0.0319(7) Uani 1 1 d . . .
H55 H 0.1577 0.9618 0.2151 0.038 Uiso 1 1 calc R . .
C56 C 0.1834(2) 1.0291(2) 0.14849(14) 0.0366(8) Uani 1 1 d . . .
H56 H 0.1647 1.0879 0.1511 0.044 Uiso 1 1 calc R . .
C57 C 0.2217(2) 0.9930(2) 0.10763(14) 0.0338(7) Uani 1 1 d . . .
H57 H 0.2324 1.0261 0.0785 0.041 Uiso 1 1 calc R . .
C58 C 0.2058(2) 0.7815(2) 0.24171(12) 0.0264(7) Uani 1 1 d . . .
C59 C 0.1428(2) 0.7169(2) 0.24697(13) 0.0291(7) Uani 1 1 d . . .
H59 H 0.1110 0.6843 0.2157 0.035 Uiso 1 1 calc R . .
C60 C 0.1265(2) 0.7001(2) 0.29797(13) 0.0318(7) Uani 1 1 d . . .
H60 H 0.0829 0.6576 0.3004 0.038 Uiso 1 1 calc R . .
C61 C 0.1751(2) 0.7466(2) 0.34577(12) 0.0284(7) Uani 1 1 d . . .
C62 C 0.2349(3) 0.8139(2) 0.34015(14) 0.0376(8) Uani 1 1 d . . .
H62 H 0.2652 0.8477 0.3712 0.045 Uiso 1 1 calc R . .
C63 C 0.2501(3) 0.8314(2) 0.28914(14) 0.0367(8) Uani 1 1 d . . .
H63 H 0.2903 0.8771 0.2862 0.044 Uiso 1 1 calc R . .
C64 C 0.2087(3) 0.7999(3) 0.45670(15) 0.0571(12) Uani 1 1 d . . .
H64A H 0.2725 0.8035 0.4577 0.086 Uiso 1 1 calc R . .
H64B H 0.2039 0.7858 0.4934 0.086 Uiso 1 1 calc R . .
H64C H 0.1794 0.8564 0.4448 0.086 Uiso 1 1 calc R . .
N1 N 0.08489(18) 0.58175(17) 0.03926(10) 0.0278(6) Uani 1 1 d . . .
N2 N 0.06459(17) 0.77243(16) 0.01857(10) 0.0248(5) Uani 1 1 d . . .
N3 N 0.20774(17) 0.86224(17) -0.01411(10) 0.0236(5) Uani 1 1 d . . .
N4 N 0.39621(18) 0.82213(18) 0.04791(10) 0.0291(6) Uani 1 1 d . . .
N5 N 0.10777(19) 0.68383(17) -0.08746(11) 0.0285(6) Uani 1 1 d . . .
N6 N 0.26360(18) 0.63897(17) 0.00620(10) 0.0248(5) Uani 1 1 d . . .
N7 N 0.26946(18) 0.71460(17) 0.11143(10) 0.0249(5) Uani 1 1 d . . .
N8 N 0.24067(18) 0.90589(17) 0.11579(10) 0.0274(6) Uani 1 1 d . . .
S1 S -0.32486(6) 0.70860(6) 0.18472(4) 0.0380(2) Uani 1 1 d . . .
S2 S 0.46218(6) 0.97935(7) -0.25354(3) 0.0371(2) Uani 1 1 d . . .
S3 S 0.49300(7) 0.56025(7) -0.25061(4) 0.0433(2) Uani 1 1 d . . .
S4 S 0.15369(7) 0.71483(6) 0.40886(4) 0.0388(2) Uani 1 1 d . . .
Zn1 Zn 0.27393(3) 0.82062(2) 0.063294(14) 0.02544(10) Uani 1 1 d . . .
Zn2 Zn 0.13195(3) 0.67164(2) -0.004726(15) 0.02633(10) Uani 1 1 d . . .


_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
C1 N1 1.336(4) . ?
C1 C2 1.409(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.357(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.423(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.395(4) . ?
C4 N1 1.404(4) . ?
C5 C6 1.406(4) . ?
C5 C10 1.486(4) . ?
C6 N2 1.390(4) . ?
C6 C7 1.428(4) . ?
C7 C8 1.380(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.423(4) . ?
C8 H8 0.9300 . ?
C9 N2 1.344(4) . ?
C9 C17 1.444(4) . ?
C10 C15 1.396(4) . ?
C10 C11 1.398(4) . ?
C11 C12 1.380(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.384(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.380(5) . ?
C13 S1 1.772(3) . ?
C14 C15 1.380(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 S1 1.798(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N3 1.351(4) . ?
C17 C18 1.415(4) . ?
C18 C19 1.367(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.418(4) . ?
C19 H19 0.9300 . ?
C20 N3 1.393(3) . ?
C20 C21 1.413(4) . ?
C21 C22 1.386(4) . ?
C21 C26 1.494(4) . ?
C22 N4 1.387(4) . ?
C22 C23 1.423(4) . ?
C23 C24 1.357(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.407(5) . ?
C24 H24 0.9300 . ?
C25 N4 1.334(4) . ?
C25 H25 0.9300 . ?
C26 C31 1.387(4) . ?
C26 C27 1.401(4) . ?
C27 C28 1.385(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.391(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.396(4) . ?
C29 S2 1.762(3) . ?
C30 C31 1.385(4) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 S2 1.788(4) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N5 1.338(4) . ?
C33 C34 1.394(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.380(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.422(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.389(4) . ?
C36 N5 1.391(4) . ?
C37 C38 1.416(4) . ?
C37 C42 1.492(4) . ?
C38 N6 1.393(4) . ?
C38 C39 1.424(4) . ?
C39 C40 1.376(4) . ?
C39 H39 0.9300 . ?
C40 C41 1.414(4) . ?
C40 H40 0.9300 . ?
C41 N6 1.353(4) . ?
C41 C49 1.441(4) . ?
C42 C47 1.392(4) . ?
C42 C43 1.394(4) . ?
C43 C44 1.362(4) . ?
C43 H43 0.9300 . ?
C44 C45 1.393(5) . ?
C44 H44 0.9300 . ?
C45 C46 1.377(5) . ?
C45 S3 1.775(3) . ?
C46 C47 1.393(4) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 S3 1.789(4) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 N7 1.354(4) . ?
C49 C50 1.415(4) . ?
C50 C51 1.365(4) . ?
C50 H50 0.9300 . ?
C51 C52 1.424(4) . ?
C51 H51 0.9300 . ?
C52 N7 1.390(4) . ?
C52 C53 1.406(4) . ?
C53 C54 1.401(4) . ?
C53 C58 1.492(4) . ?
C54 N8 1.403(4) . ?
C54 C55 1.426(4) . ?
C55 C56 1.378(4) . ?
C55 H55 0.9300 . ?
C56 C57 1.412(5) . ?
C56 H56 0.9300 . ?
C57 N8 1.335(4) . ?
C57 H57 0.9300 . ?
C58 C59 1.389(4) . ?
C58 C63 1.398(4) . ?
C59 C60 1.383(4) . ?
C59 H59 0.9300 . ?
C60 C61 1.395(4) . ?
C60 H60 0.9300 . ?
C61 C62 1.385(4) . ?
C61 S4 1.757(3) . ?
C62 C63 1.379(4) . ?
C62 H62 0.9300 . ?
C63 H63 0.9300 . ?
C64 S4 1.780(4) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
N1 Zn2 1.987(2) . ?
N2 Zn2 1.994(2) . ?
N3 Zn1 2.004(2) . ?
N4 Zn1 1.993(3) . ?
N5 Zn2 1.997(3) . ?
N6 Zn2 1.994(3) . ?
N7 Zn1 1.998(2) . ?
N8 Zn1 1.989(2) . ?

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 C1 C2 110.5(3) . . ?
N1 C1 H1 124.7 . . ?
C2 C1 H1 124.7 . . ?
C3 C2 C1 107.6(3) . . ?
C3 C2 H2 126.2 . . ?
C1 C2 H2 126.2 . . ?
C2 C3 C4 106.9(3) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
C5 C4 N1 124.0(3) . . ?
C5 C4 C3 127.8(3) . . ?
N1 C4 C3 108.2(3) . . ?
C4 C5 C6 125.4(3) . . ?
C4 C5 C10 117.6(3) . . ?
C6 C5 C10 116.9(3) . . ?
N2 C6 C5 125.4(3) . . ?
N2 C6 C7 108.6(3) . . ?
C5 C6 C7 125.9(3) . . ?
C8 C7 C6 107.3(3) . . ?
C8 C7 H7 126.4 . . ?
C6 C7 H7 126.4 . . ?
C7 C8 C9 106.0(3) . . ?
C7 C8 H8 127.0 . . ?
C9 C8 H8 127.0 . . ?
N2 C9 C8 111.1(3) . . ?
N2 C9 C17 120.9(3) . . ?
C8 C9 C17 128.1(3) . . ?
C15 C10 C11 118.1(3) . . ?
C15 C10 C5 120.2(3) . . ?
C11 C10 C5 121.7(3) . . ?
C12 C11 C10 120.2(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 121.2(3) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C14 C13 C12 118.8(3) . . ?
C14 C13 S1 122.1(3) . . ?
C12 C13 S1 119.0(2) . . ?
C13 C14 C15 120.5(3) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C10 121.0(3) . . ?
C14 C15 H15 119.5 . . ?
C10 C15 H15 119.5 . . ?
S1 C16 H16A 109.5 . . ?
S1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C18 110.8(3) . . ?
N3 C17 C9 120.6(3) . . ?
C18 C17 C9 128.5(3) . . ?
C19 C18 C17 106.1(3) . . ?
C19 C18 H18 126.9 . . ?
C17 C18 H18 126.9 . . ?
C18 C19 C20 108.1(3) . . ?
C18 C19 H19 125.9 . . ?
C20 C19 H19 125.9 . . ?
N3 C20 C21 124.5(3) . . ?
N3 C20 C19 108.1(3) . . ?
C21 C20 C19 127.4(3) . . ?
C22 C21 C20 125.8(3) . . ?
C22 C21 C26 117.5(3) . . ?
C20 C21 C26 116.5(3) . . ?
C21 C22 N4 124.6(3) . . ?
C21 C22 C23 127.3(3) . . ?
N4 C22 C23 108.0(3) . . ?
C24 C23 C22 107.5(3) . . ?
C24 C23 H23 126.2 . . ?
C22 C23 H23 126.2 . . ?
C23 C24 C25 106.5(3) . . ?
C23 C24 H24 126.8 . . ?
C25 C24 H24 126.8 . . ?
N4 C25 C24 111.1(3) . . ?
N4 C25 H25 124.4 . . ?
C24 C25 H25 124.4 . . ?
C31 C26 C27 118.2(3) . . ?
C31 C26 C21 122.5(3) . . ?
C27 C26 C21 119.2(3) . . ?
C28 C27 C26 120.7(3) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 120.7(3) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C28 C29 C30 118.9(3) . . ?
C28 C29 S2 115.8(2) . . ?
C30 C29 S2 125.3(2) . . ?
C31 C30 C29 120.0(3) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C26 121.5(3) . . ?
C30 C31 H31 119.2 . . ?
C26 C31 H31 119.2 . . ?
S2 C32 H32A 109.5 . . ?
S2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
S2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N5 C33 C34 111.8(3) . . ?
N5 C33 H33 124.1 . . ?
C34 C33 H33 124.1 . . ?
C35 C34 C33 106.3(3) . . ?
C35 C34 H34 126.9 . . ?
C33 C34 H34 126.9 . . ?
C34 C35 C36 107.2(3) . . ?
C34 C35 H35 126.4 . . ?
C36 C35 H35 126.4 . . ?
C37 C36 N5 125.0(3) . . ?
C37 C36 C35 126.8(3) . . ?
N5 C36 C35 108.1(3) . . ?
C36 C37 C38 126.2(3) . . ?
C36 C37 C42 118.1(3) . . ?
C38 C37 C42 115.7(3) . . ?
N6 C38 C37 123.4(3) . . ?
N6 C38 C39 108.5(3) . . ?
C37 C38 C39 128.0(3) . . ?
C40 C39 C38 107.6(3) . . ?
C40 C39 H39 126.2 . . ?
C38 C39 H39 126.2 . . ?
C39 C40 C41 106.1(3) . . ?
C39 C40 H40 127.0 . . ?
C41 C40 H40 127.0 . . ?
N6 C41 C40 111.2(3) . . ?
N6 C41 C49 119.1(3) . . ?
C40 C41 C49 129.5(3) . . ?
C47 C42 C43 117.8(3) . . ?
C47 C42 C37 120.6(3) . . ?
C43 C42 C37 121.6(3) . . ?
C44 C43 C42 121.9(3) . . ?
C44 C43 H43 119.0 . . ?
C42 C43 H43 119.0 . . ?
C43 C44 C45 120.1(3) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C46 C45 C44 119.3(3) . . ?
C46 C45 S3 117.8(3) . . ?
C44 C45 S3 122.9(2) . . ?
C45 C46 C47 120.4(3) . . ?
C45 C46 H46 119.8 . . ?
C47 C46 H46 119.8 . . ?
C42 C47 C46 120.5(3) . . ?
C42 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
S3 C48 H48A 109.5 . . ?
S3 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
S3 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N7 C49 C50 111.0(3) . . ?
N7 C49 C41 119.5(3) . . ?
C50 C49 C41 129.4(3) . . ?
C51 C50 C49 106.1(3) . . ?
C51 C50 H50 127.0 . . ?
C49 C50 H50 127.0 . . ?
C50 C51 C52 108.2(3) . . ?
C50 C51 H51 125.9 . . ?
C52 C51 H51 125.9 . . ?
N7 C52 C53 124.6(3) . . ?
N7 C52 C51 108.0(3) . . ?
C53 C52 C51 127.2(3) . . ?
C54 C53 C52 126.2(3) . . ?
C54 C53 C58 118.3(3) . . ?
C52 C53 C58 115.5(3) . . ?
C53 C54 N8 124.2(3) . . ?
C53 C54 C55 127.8(3) . . ?
N8 C54 C55 107.9(3) . . ?
C56 C55 C54 107.8(3) . . ?
C56 C55 H55 126.1 . . ?
C54 C55 H55 126.1 . . ?
C55 C56 C57 105.6(3) . . ?
C55 C56 H56 127.2 . . ?
C57 C56 H56 127.2 . . ?
N8 C57 C56 112.1(3) . . ?
N8 C57 H57 123.9 . . ?
C56 C57 H57 123.9 . . ?
C59 C58 C63 118.0(3) . . ?
C59 C58 C53 120.7(3) . . ?
C63 C58 C53 121.2(3) . . ?
C60 C59 C58 121.2(3) . . ?
C60 C59 H59 119.4 . . ?
C58 C59 H59 119.4 . . ?
C59 C60 C61 120.3(3) . . ?
C59 C60 H60 119.8 . . ?
C61 C60 H60 119.8 . . ?
C62 C61 C60 118.5(3) . . ?
C62 C61 S4 125.2(3) . . ?
C60 C61 S4 116.2(2) . . ?
C63 C62 C61 121.0(3) . . ?
C63 C62 H62 119.5 . . ?
C61 C62 H62 119.5 . . ?
C62 C63 C58 120.8(3) . . ?
C62 C63 H63 119.6 . . ?
C58 C63 H63 119.6 . . ?
S4 C64 H64A 109.5 . . ?
S4 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
S4 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C1 N1 C4 106.7(3) . . ?
C1 N1 Zn2 127.3(2) . . ?
C4 N1 Zn2 125.2(2) . . ?
C9 N2 C6 107.0(2) . . ?
C9 N2 Zn2 123.6(2) . . ?
C6 N2 Zn2 122.0(2) . . ?
C17 N3 C20 106.8(2) . . ?
C17 N3 Zn1 125.7(2) . . ?
C20 N3 Zn1 122.5(2) . . ?
C25 N4 C22 106.8(3) . . ?
C25 N4 Zn1 126.0(2) . . ?
C22 N4 Zn1 125.2(2) . . ?
C33 N5 C36 106.7(3) . . ?
C33 N5 Zn2 127.5(2) . . ?
C36 N5 Zn2 124.9(2) . . ?
C41 N6 C38 106.5(2) . . ?
C41 N6 Zn2 124.4(2) . . ?
C38 N6 Zn2 124.2(2) . . ?
C49 N7 C52 106.7(2) . . ?
C49 N7 Zn1 125.6(2) . . ?
C52 N7 Zn1 124.6(2) . . ?
C57 N8 C54 106.5(3) . . ?
C57 N8 Zn1 127.4(2) . . ?
C54 N8 Zn1 125.0(2) . . ?
C13 S1 C16 100.96(18) . . ?
C29 S2 C32 103.83(16) . . ?
C45 S3 C48 101.59(17) . . ?
C61 S4 C64 103.66(17) . . ?
N8 Zn1 N4 122.69(11) . . ?
N8 Zn1 N7 93.16(10) . . ?
N4 Zn1 N7 108.35(11) . . ?
N8 Zn1 N3 106.45(10) . . ?
N4 Zn1 N3 92.91(10) . . ?
N7 Zn1 N3 136.92(10) . . ?
N1 Zn2 N2 93.28(10) . . ?
N1 Zn2 N6 105.03(10) . . ?
N2 Zn2 N6 135.92(11) . . ?
N1 Zn2 N5 129.83(11) . . ?
N2 Zn2 N5 105.76(10) . . ?
N6 Zn2 N5 92.76(10) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        30.09
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.103
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound5a
_database_code_depnum_ccdc_archive 'CCDC 1040039'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C96 H72 N12 S6 Zn3), C5 H12, 2(C4 H8 O2) '
_chemical_formula_sum            'C205 H172 N24 O4 S12 Zn6'
_chemical_formula_weight         3812.61

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'
S S 0.1246 0.1234 '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           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   13.3649(5)
_cell_length_b                   18.2896(6)
_cell_length_c                   18.8109(7)
_cell_angle_alpha                96.448(2)
_cell_angle_beta                 99.538(2)
_cell_angle_gamma                94.693(2)
_cell_volume                     4482.1(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9715
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      24.20

_exptl_crystal_description       rod
_exptl_crystal_colour            dark-green
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1974
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8732
_exptl_absorpt_correction_T_max  0.9708
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
The n-Pentane molecule is disordered over two positions. 
The hydrogen atoms on this molecule have not been introduced
 but are taken into account in the compound formula. 
EADP as well as DFIX constraints have been used on the 
n-pentane molecule as well as on the ethyl acetate.
Two methyl groups of SMe functions of the ligands are 
disordered over two positions. This has been modeled using 
the PART command.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            81271
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_sigmaI/netI    0.1076
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.11
_diffrn_reflns_theta_max         29.43
_reflns_number_total             24097
_reflns_number_gt                13325
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0998P)²+1.8278P] 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         24097
_refine_ls_number_parameters     1117
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.2003
_refine_ls_wR_factor_gt          0.1602
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.023
_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
C1 C 0.9539(3) 0.6615(3) -0.0901(2) 0.0304(10) Uani 1 1 d . . .
H1 H 0.9282 0.6157 -0.1161 0.037 Uiso 1 1 calc R . .
C2 C 1.0148(4) 0.7147(3) -0.1157(2) 0.0346(11) Uani 1 1 d . . .
H2 H 1.0360 0.7108 -0.1605 0.042 Uiso 1 1 calc R . .
C3 C 1.0372(3) 0.7735(3) -0.0625(2) 0.0288(10) Uani 1 1 d . . .
H3 H 1.0770 0.8173 -0.0639 0.035 Uiso 1 1 calc R . .
C4 C 0.9881(3) 0.7552(2) -0.0042(2) 0.0254(9) Uani 1 1 d . . .
C5 C 0.9815(3) 0.8018(2) 0.0592(2) 0.0240(9) Uani 1 1 d . . .
C6 C 0.9186(3) 0.7874(2) 0.1103(2) 0.0225(9) Uani 1 1 d . . .
C7 C 0.9063(3) 0.8373(2) 0.1714(2) 0.0271(9) Uani 1 1 d . . .
H7 H 0.9368 0.8856 0.1839 0.033 Uiso 1 1 calc R . .
C8 C 0.8416(3) 0.8012(2) 0.2084(2) 0.0266(9) Uani 1 1 d . . .
H8 H 0.8193 0.8204 0.2503 0.032 Uiso 1 1 calc R . .
C9 C 0.8154(3) 0.7289(2) 0.1704(2) 0.0215(8) Uani 1 1 d . . .
C10 C 1.0504(3) 0.8713(2) 0.0737(2) 0.0272(9) Uani 1 1 d . . .
C11 C 1.1554(3) 0.8679(2) 0.0818(2) 0.0302(10) Uani 1 1 d . . .
H11 H 1.1802 0.8218 0.0806 0.036 Uiso 1 1 calc R . .
C12 C 1.2231(4) 0.9300(3) 0.0916(2) 0.0328(10) Uani 1 1 d . . .
H12 H 1.2928 0.9258 0.0969 0.039 Uiso 1 1 calc R . .
C13 C 1.1868(4) 1.0002(3) 0.0934(2) 0.0325(10) Uani 1 1 d . . .
C14 C 1.0834(4) 1.0047(3) 0.0875(3) 0.0352(11) Uani 1 1 d . . .
H14 H 1.0586 1.0508 0.0906 0.042 Uiso 1 1 calc R . .
C15 C 1.0161(3) 0.9408(2) 0.0767(2) 0.0309(10) Uani 1 1 d . . .
H15 H 0.9464 0.9448 0.0715 0.037 Uiso 1 1 calc R . .
C16 C 1.2109(5) 1.1535(3) 0.1162(4) 0.0589(16) Uani 1 1 d . . .
H16A H 1.1654 1.1578 0.0721 0.088 Uiso 1 1 calc R . .
H16B H 1.2574 1.1976 0.1299 0.088 Uiso 1 1 calc R . .
H16C H 1.1723 1.1469 0.1542 0.088 Uiso 1 1 calc R . .
C17 C 0.7507(3) 0.6695(2) 0.1903(2) 0.0212(8) Uani 1 1 d . . .
C18 C 0.6851(3) 0.6144(2) 0.1420(2) 0.0244(9) Uani 1 1 d . . .
H18 H 0.6739 0.6101 0.0915 0.029 Uiso 1 1 calc R . .
C19 C 0.6416(3) 0.5692(2) 0.1830(2) 0.0224(9) Uani 1 1 d . . .
H19 H 0.5953 0.5277 0.1659 0.027 Uiso 1 1 calc R . .
C20 C 0.6800(3) 0.5968(2) 0.2573(2) 0.0197(8) Uani 1 1 d . . .
C21 C 0.6549(3) 0.5640(2) 0.3176(2) 0.0207(8) Uani 1 1 d . . .
C22 C 0.6765(3) 0.5965(2) 0.3902(2) 0.0226(9) Uani 1 1 d . . .
C23 C 0.6586(3) 0.5655(3) 0.4530(2) 0.0301(10) Uani 1 1 d . . .
H23 H 0.6289 0.5179 0.4543 0.036 Uiso 1 1 calc R . .
C24 C 0.6933(4) 0.6185(3) 0.5120(2) 0.0372(11) Uani 1 1 d . . .
H24 H 0.6911 0.6139 0.5605 0.045 Uiso 1 1 calc R . .
C25 C 0.7322(3) 0.6800(3) 0.4845(2) 0.0295(10) Uani 1 1 d . . .
H25 H 0.7612 0.7240 0.5129 0.035 Uiso 1 1 calc R . .
C26 C 0.6053(3) 0.4870(2) 0.3016(2) 0.0219(9) Uani 1 1 d . . .
C27 C 0.6463(3) 0.4340(2) 0.2581(2) 0.0270(9) Uani 1 1 d . . .
H27 H 0.7046 0.4477 0.2398 0.032 Uiso 1 1 calc R . .
C28 C 0.6019(3) 0.3618(2) 0.2419(2) 0.0302(10) Uani 1 1 d . . .
H28 H 0.6297 0.3276 0.2124 0.036 Uiso 1 1 calc R . .
C29 C 0.5160(3) 0.3405(3) 0.2698(2) 0.0313(10) Uani 1 1 d . . .
C30 C 0.4746(3) 0.3917(3) 0.3127(2) 0.0313(10) Uani 1 1 d . . .
H30 H 0.4168 0.3772 0.3312 0.038 Uiso 1 1 calc R . .
C31 C 0.5173(3) 0.4644(2) 0.3285(2) 0.0268(10) Uani 1 1 d . . .
H31 H 0.4878 0.4984 0.3571 0.032 Uiso 1 1 calc R . .
C32 C 0.5223(5) 0.2021(3) 0.1916(4) 0.073(2) Uani 1 1 d . . .
H32A H 0.5169 0.2240 0.1473 0.110 Uiso 1 1 calc R . .
H32B H 0.4952 0.1511 0.1812 0.110 Uiso 1 1 calc R . .
H32C H 0.5927 0.2056 0.2143 0.110 Uiso 1 1 calc R . .
C33 C 0.6937(3) 0.6014(3) -0.0903(2) 0.0277(10) Uani 1 1 d . . .
H33 H 0.7049 0.6485 -0.1036 0.033 Uiso 1 1 calc R . .
C34 C 0.6251(3) 0.5449(3) -0.1315(2) 0.0309(10) Uani 1 1 d . . .
H34 H 0.5839 0.5471 -0.1760 0.037 Uiso 1 1 calc R . .
C35 C 0.6306(3) 0.4852(3) -0.0932(2) 0.0283(10) Uani 1 1 d . . .
H35 H 0.5933 0.4391 -0.1070 0.034 Uiso 1 1 calc R . .
C36 C 0.7036(3) 0.5067(2) -0.0287(2) 0.0229(9) Uani 1 1 d . . .
C37 C 0.7372(3) 0.4634(2) 0.0257(2) 0.0207(8) Uani 1 1 d . . .
C38 C 0.8240(3) 0.4818(2) 0.0811(2) 0.0207(8) Uani 1 1 d . . .
C39 C 0.8519(3) 0.4414(2) 0.1414(2) 0.0249(9) Uani 1 1 d . . .
H39 H 0.8147 0.4001 0.1523 0.030 Uiso 1 1 calc R . .
C40 C 0.9432(3) 0.4748(2) 0.1799(2) 0.0246(9) Uani 1 1 d . . .
H40 H 0.9793 0.4611 0.2222 0.030 Uiso 1 1 calc R . .
C41 C 0.9721(3) 0.5344(2) 0.1428(2) 0.0218(9) Uani 1 1 d . . .
C42 C 0.6759(3) 0.3913(2) 0.0235(2) 0.0227(9) Uani 1 1 d . . .
C43 C 0.7207(3) 0.3247(2) 0.0225(2) 0.0280(10) Uani 1 1 d . . .
H43 H 0.7913 0.3257 0.0287 0.034 Uiso 1 1 calc R . .
C44 C 0.6615(3) 0.2575(2) 0.0124(2) 0.0306(10) Uani 1 1 d . . .
H44 H 0.6926 0.2138 0.0112 0.037 Uiso 1 1 calc R . .
C45 C 0.5552(3) 0.2548(3) 0.0040(2) 0.0314(10) Uani 1 1 d . . .
C46 C 0.5109(4) 0.3205(3) 0.0083(3) 0.0356(11) Uani 1 1 d . . .
H46 H 0.4406 0.3196 0.0047 0.043 Uiso 1 1 calc R . .
C47 C 0.5706(3) 0.3878(3) 0.0179(2) 0.0315(10) Uani 1 1 d . . .
H47 H 0.5395 0.4315 0.0208 0.038 Uiso 1 1 calc R . .
C48 C 0.3591(4) 0.1861(3) -0.0452(4) 0.0603(17) Uani 1 1 d . . .
H48A H 0.3339 0.2136 -0.0066 0.090 Uiso 1 1 calc R . .
H48B H 0.3162 0.1406 -0.0612 0.090 Uiso 1 1 calc R . .
H48C H 0.3588 0.2147 -0.0850 0.090 Uiso 1 1 calc R . .
C49 C 1.0684(3) 0.5801(2) 0.1566(2) 0.0217(8) Uani 1 1 d . . .
C50 C 1.1048(3) 0.6259(2) 0.1078(2) 0.0289(10) Uani 1 1 d . . .
H50 H 1.0715 0.6315 0.0615 0.035 Uiso 1 1 calc R . .
C51 C 1.1971(3) 0.6598(2) 0.1417(2) 0.0276(9) Uani 1 1 d . . .
H51 H 1.2384 0.6933 0.1230 0.033 Uiso 1 1 calc R . .
C52 C 1.2196(3) 0.6349(2) 0.2111(2) 0.0228(9) Uani 1 1 d . . .
C53 C 1.3087(3) 0.6584(2) 0.2618(2) 0.0257(9) Uani 1 1 d . . .
C54 C 1.3396(3) 0.6311(2) 0.3284(2) 0.0259(9) Uani 1 1 d . . .
C55 C 1.4198(3) 0.6610(3) 0.3861(2) 0.0343(11) Uani 1 1 d . . .
H55 H 1.4675 0.7008 0.3857 0.041 Uiso 1 1 calc R . .
C56 C 1.4143(4) 0.6205(3) 0.4423(3) 0.0400(12) Uani 1 1 d . . .
H56 H 1.4571 0.6272 0.4874 0.048 Uiso 1 1 calc R . .
C57 C 1.3316(3) 0.5669(3) 0.4186(2) 0.0342(11) Uani 1 1 d . . .
H57 H 1.3104 0.5319 0.4466 0.041 Uiso 1 1 calc R . .
C58 C 1.3744(3) 0.7223(2) 0.2463(2) 0.0260(9) Uani 1 1 d . . .
C59 C 1.4768(3) 0.7180(3) 0.2416(3) 0.0354(11) Uani 1 1 d . . .
H59 H 1.5042 0.6732 0.2451 0.042 Uiso 1 1 calc R . .
C60 C 1.5382(4) 0.7790(3) 0.2317(3) 0.0399(12) Uani 1 1 d . . .
H60 H 1.6061 0.7745 0.2282 0.048 Uiso 1 1 calc R . .
C61 C 1.5006(3) 0.8468(3) 0.2271(2) 0.0334(11) Uani 1 1 d . A .
C62 C 1.3976(4) 0.8514(3) 0.2307(3) 0.0406(12) Uani 1 1 d . . .
H62 H 1.3704 0.8962 0.2270 0.049 Uiso 1 1 calc R . .
C63 C 1.3363(3) 0.7905(3) 0.2398(3) 0.0360(11) Uani 1 1 d . . .
H63 H 1.2679 0.7948 0.2416 0.043 Uiso 1 1 calc R . .
C64 C 1.534(2) 0.9974(10) 0.254(2) 0.074(9) Uani 0.40(3) 1 d P A 1
H64A H 1.4682 0.9998 0.2249 0.112 Uiso 0.40(3) 1 calc PR A 1
H64B H 1.5774 1.0416 0.2525 0.112 Uiso 0.40(3) 1 calc PR A 1
H64C H 1.5267 0.9928 0.3029 0.112 Uiso 0.40(3) 1 calc PR A 1
C64B C 1.5080(9) 0.9946(7) 0.1956(16) 0.074(7) Uani 0.60(3) 1 d P A 2
H64D H 1.4639 0.9787 0.1498 0.111 Uiso 0.60(3) 1 calc PR A 2
H64E H 1.5505 1.0385 0.1920 0.111 Uiso 0.60(3) 1 calc PR A 2
H64F H 1.4676 1.0050 0.2325 0.111 Uiso 0.60(3) 1 calc PR A 2
C65 C 1.2119(3) 0.3790(3) 0.2638(2) 0.0338(11) Uani 1 1 d . . .
H65 H 1.2625 0.3976 0.2403 0.041 Uiso 1 1 calc R . .
C66 C 1.1909(4) 0.3045(3) 0.2707(3) 0.0375(11) Uani 1 1 d . . .
H66 H 1.2247 0.2656 0.2535 0.045 Uiso 1 1 calc R . .
C67 C 1.1116(4) 0.2996(3) 0.3071(2) 0.0318(10) Uani 1 1 d . . .
H67 H 1.0802 0.2564 0.3189 0.038 Uiso 1 1 calc R . .
C68 C 1.0854(3) 0.3724(2) 0.3238(2) 0.0236(9) Uani 1 1 d . . .
C69 C 1.0087(3) 0.3953(2) 0.3620(2) 0.0238(9) Uani 1 1 d . . .
C70 C 0.9873(3) 0.4686(2) 0.3807(2) 0.0218(9) Uani 1 1 d . . .
C71 C 0.9110(3) 0.4907(2) 0.4203(2) 0.0267(9) Uani 1 1 d . . .
H71 H 0.8665 0.4592 0.4389 0.032 Uiso 1 1 calc R . .
C72 C 0.9138(3) 0.5652(2) 0.4264(2) 0.0263(9) Uani 1 1 d . . .
H72 H 0.8722 0.5945 0.4497 0.032 Uiso 1 1 calc R . .
C73 C 0.9940(3) 0.5899(2) 0.3899(2) 0.0233(9) Uani 1 1 d . . .
C74 C 0.9400(3) 0.3348(2) 0.3820(2) 0.0253(9) Uani 1 1 d . . .
C75 C 0.9771(3) 0.2844(2) 0.4270(2) 0.0300(10) Uani 1 1 d . . .
H75 H 1.0459 0.2896 0.4476 0.036 Uiso 1 1 calc R . .
C76 C 0.9144(4) 0.2273(3) 0.4417(3) 0.0373(11) Uani 1 1 d . . .
H76 H 0.9411 0.1941 0.4720 0.045 Uiso 1 1 calc R . .
C77 C 0.8112(4) 0.2183(3) 0.4117(3) 0.0389(12) Uani 1 1 d . B .
C78 C 0.7729(4) 0.2686(3) 0.3684(3) 0.0437(13) Uani 1 1 d . . .
H78 H 0.7037 0.2640 0.3489 0.052 Uiso 1 1 calc R . .
C79 C 0.8364(3) 0.3259(3) 0.3537(3) 0.0402(12) Uani 1 1 d . . .
H79 H 0.8093 0.3594 0.3240 0.048 Uiso 1 1 calc R . .
C80 C 0.5987(15) 0.1704(13) 0.4130(14) 0.090(5) Uani 0.417(14) 1 d P B 3
H80A H 0.5833 0.1785 0.3629 0.135 Uiso 0.417(14) 1 calc PR B 3
H80B H 0.5932 0.2150 0.4436 0.135 Uiso 0.417(14) 1 calc PR B 3
H80C H 0.5514 0.1315 0.4218 0.135 Uiso 0.417(14) 1 calc PR B 3
C80B C 0.6320(11) 0.1310(9) 0.3673(10) 0.090(5) Uani 0.583(14) 1 d P B 4
H80D H 0.5966 0.1745 0.3700 0.135 Uiso 0.583(14) 1 calc PR B 4
H80E H 0.5877 0.0891 0.3735 0.135 Uiso 0.583(14) 1 calc PR B 4
H80F H 0.6527 0.1230 0.3208 0.135 Uiso 0.583(14) 1 calc PR B 4
C81 C 1.0297(3) 0.6652(2) 0.3848(2) 0.0237(9) Uani 1 1 d . . .
C82 C 1.1323(3) 0.6944(2) 0.3880(2) 0.0309(10) Uani 1 1 d . . .
H82 H 1.1893 0.6682 0.3933 0.037 Uiso 1 1 calc R . .
C83 C 1.1317(3) 0.7676(2) 0.3819(2) 0.0300(10) Uani 1 1 d . . .
H83 H 1.1884 0.8007 0.3821 0.036 Uiso 1 1 calc R . .
C84 C 1.0288(3) 0.7845(2) 0.3751(2) 0.0263(9) Uani 1 1 d . . .
C85 C 0.9966(3) 0.8560(2) 0.3752(2) 0.0266(9) Uani 1 1 d . . .
C86 C 0.8990(3) 0.8757(2) 0.3832(2) 0.0270(9) Uani 1 1 d . . .
C87 C 0.8645(4) 0.9472(3) 0.3888(2) 0.0345(11) Uani 1 1 d . . .
H87 H 0.9033 0.9916 0.3882 0.041 Uiso 1 1 calc R . .
C88 C 0.7638(4) 0.9391(3) 0.3954(3) 0.0422(12) Uani 1 1 d . . .
H88 H 0.7216 0.9765 0.4013 0.051 Uiso 1 1 calc R . .
C89 C 0.7373(4) 0.8628(3) 0.3912(2) 0.0337(11) Uani 1 1 d . . .
H89 H 0.6721 0.8416 0.3926 0.040 Uiso 1 1 calc R . .
C90 C 1.0744(3) 0.9156(2) 0.3660(2) 0.0276(9) Uani 1 1 d . . .
C91 C 1.1076(4) 0.9770(3) 0.4179(2) 0.0353(11) Uani 1 1 d . . .
H91 H 1.0826 0.9807 0.4613 0.042 Uiso 1 1 calc R . .
C92 C 1.1765(4) 1.0323(3) 0.4060(3) 0.0373(12) Uani 1 1 d . . .
H92 H 1.1980 1.0725 0.4416 0.045 Uiso 1 1 calc R . .
C93 C 1.2148(4) 1.0288(3) 0.3412(3) 0.0360(11) Uani 1 1 d . . .
C94 C 1.1835(4) 0.9673(3) 0.2897(3) 0.0356(11) Uani 1 1 d . . .
H94 H 1.2086 0.9638 0.2463 0.043 Uiso 1 1 calc R . .
C95 C 1.1159(3) 0.9118(2) 0.3023(2) 0.0300(10) Uani 1 1 d . . .
H95 H 1.0971 0.8704 0.2675 0.036 Uiso 1 1 calc R . .
C96 C 1.3175(6) 1.1673(3) 0.3948(3) 0.070(2) Uani 1 1 d . . .
H96A H 1.2522 1.1832 0.4005 0.105 Uiso 1 1 calc R . .
H96B H 1.3616 1.2086 0.3869 0.105 Uiso 1 1 calc R . .
H96C H 1.3470 1.1479 0.4379 0.105 Uiso 1 1 calc R . .
N1 N 0.9372(3) 0.6844(2) -0.02360(18) 0.0256(8) Uani 1 1 d . . .
N2 N 0.8592(2) 0.72071(19) 0.11098(17) 0.0228(7) Uani 1 1 d . . .
N3 N 0.7454(2) 0.66027(18) 0.25985(17) 0.0198(7) Uani 1 1 d . . .
N4 N 0.7227(2) 0.66796(19) 0.41183(18) 0.0231(7) Uani 1 1 d . . .
N5 N 0.7416(2) 0.57944(19) -0.02872(17) 0.0227(7) Uani 1 1 d . . .
N6 N 0.8991(2) 0.53985(18) 0.08445(17) 0.0218(7) Uani 1 1 d . . .
N7 N 1.1389(2) 0.58448(19) 0.21819(17) 0.0229(7) Uani 1 1 d . . .
N8 N 1.2863(3) 0.5722(2) 0.35026(19) 0.0262(8) Uani 1 1 d . . .
N9 N 1.1491(3) 0.4205(2) 0.29581(18) 0.0257(8) Uani 1 1 d . . .
N10 N 1.0387(2) 0.53162(18) 0.36329(17) 0.0215(7) Uani 1 1 d . . .
N11 N 0.9671(3) 0.71917(18) 0.37764(18) 0.0235(7) Uani 1 1 d . . .
N12 N 0.8163(3) 0.82439(19) 0.38498(19) 0.0267(8) Uani 1 1 d . . .
S1 S 1.28089(11) 1.07588(7) 0.10246(8) 0.0476(3) Uani 1 1 d . . .
S2 S 0.45227(11) 0.24982(8) 0.25129(8) 0.0491(4) Uani 1 1 d . . .
S3 S 0.48596(11) 0.16651(7) -0.01327(8) 0.0486(4) Uani 1 1 d . . .
S4 S 1.58700(11) 0.92231(8) 0.21911(8) 0.0500(4) Uani 1 1 d . . .
S5 S 0.73722(14) 0.14246(9) 0.43434(10) 0.0662(5) Uani 1 1 d . . .
S6 S 1.30174(12) 1.09739(8) 0.31899(8) 0.0509(4) Uani 1 1 d . . .
Zn1 Zn 0.86209(3) 0.63066(3) 0.04040(2) 0.02208(12) Uani 1 1 d . . .
Zn2 Zn 1.14765(3) 0.52956(3) 0.30370(2) 0.02339(12) Uani 1 1 d . . .
Zn3 Zn 0.81548(3) 0.71666(3) 0.35485(2) 0.02258(12) Uani 1 1 d . . .
C97 C 0.6960(11) 0.0407(9) 0.0806(8) 0.216(2) Uani 1 1 d D . .
H97A H 0.6273 0.0357 0.0895 0.324 Uiso 1 1 calc R . .
H97B H 0.7146 -0.0070 0.0638 0.324 Uiso 1 1 calc R . .
H97C H 0.7008 0.0731 0.0443 0.324 Uiso 1 1 calc R . .
C98 C 0.7590(13) 0.0688(10) 0.1420(9) 0.216(2) Uani 1 1 d D . .
C99 C 0.8863(11) 0.1202(8) 0.2472(8) 0.216(2) Uani 1 1 d D . .
H99A H 0.8931 0.1727 0.2431 0.259 Uiso 1 1 calc R . .
H99B H 0.8354 0.1098 0.2769 0.259 Uiso 1 1 calc R . .
C100 C 0.9842(10) 0.0946(8) 0.2760(8) 0.216(2) Uani 1 1 d D . .
H10A H 0.9746 0.0427 0.2797 0.324 Uiso 1 1 calc R . .
H10B H 1.0105 0.1212 0.3233 0.324 Uiso 1 1 calc R . .
H10C H 1.0316 0.1033 0.2440 0.324 Uiso 1 1 calc R . .
O1 O 0.7304(8) 0.1069(6) 0.1928(6) 0.216(2) Uani 1 1 d D . .
O2 O 0.8607(8) 0.0741(6) 0.1731(6) 0.216(2) Uani 1 1 d D . .
C101 C 0.5000 0.0000 0.5000 0.186(6) Uani 1 2 d SD . .
C102 C 0.4340(10) -0.0997(9) 0.4231(6) 0.186(6) Uani 1 1 d D . .
C103 C 0.4186(13) -0.0298(11) 0.4486(11) 0.186(6) Uani 0.50 1 d PD . .
C104 C 0.5265(12) -0.0652(9) 0.4683(12) 0.186(6) Uani 0.50 1 d PD . .


_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
C1 N1 1.334(5) . ?
C1 C2 1.395(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.361(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.424(6) . ?
C3 H3 0.9300 . ?
C4 N1 1.393(5) . ?
C4 C5 1.406(6) . ?
C5 C6 1.411(6) . ?
C5 C10 1.479(6) . ?
C6 N2 1.402(5) . ?
C6 C7 1.424(6) . ?
C7 C8 1.370(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.418(6) . ?
C8 H8 0.9300 . ?
C9 N2 1.345(5) . ?
C9 C17 1.453(6) . ?
C10 C15 1.385(6) . ?
C10 C11 1.393(6) . ?
C11 C12 1.370(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.407(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.378(7) . ?
C13 S1 1.766(5) . ?
C14 C15 1.389(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 S1 1.781(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N3 1.351(5) . ?
C17 C18 1.412(5) . ?
C18 C19 1.353(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.426(5) . ?
C19 H19 0.9300 . ?
C20 N3 1.385(5) . ?
C20 C21 1.418(5) . ?
C21 C22 1.400(5) . ?
C21 C26 1.483(6) . ?
C22 N4 1.385(5) . ?
C22 C23 1.414(6) . ?
C23 C24 1.378(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.389(7) . ?
C24 H24 0.9300 . ?
C25 N4 1.344(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.403(6) . ?
C26 C31 1.405(6) . ?
C27 C28 1.383(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.385(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.379(6) . ?
C29 S2 1.771(5) . ?
C30 C31 1.383(6) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 S2 1.777(7) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N5 1.347(5) . ?
C33 C34 1.392(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.375(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.419(5) . ?
C35 H35 0.9300 . ?
C36 N5 1.384(5) . ?
C36 C37 1.402(6) . ?
C37 C38 1.415(5) . ?
C37 C42 1.487(6) . ?
C38 N6 1.388(5) . ?
C38 C39 1.438(6) . ?
C39 C40 1.368(6) . ?
C39 H39 0.9300 . ?
C40 C41 1.420(6) . ?
C40 H40 0.9300 . ?
C41 N6 1.361(5) . ?
C41 C49 1.445(6) . ?
C42 C47 1.390(6) . ?
C42 C43 1.400(6) . ?
C43 C44 1.382(6) . ?
C43 H43 0.9300 . ?
C44 C45 1.399(6) . ?
C44 H44 0.9300 . ?
C45 C46 1.384(7) . ?
C45 S3 1.762(5) . ?
C46 C47 1.387(6) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 S3 1.782(6) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 N7 1.358(5) . ?
C49 C50 1.426(6) . ?
C50 C51 1.356(6) . ?
C50 H50 0.9300 . ?
C51 C52 1.423(6) . ?
C51 H51 0.9300 . ?
C52 N7 1.394(5) . ?
C52 C53 1.400(6) . ?
C53 C54 1.410(6) . ?
C53 C58 1.488(6) . ?
C54 N8 1.382(5) . ?
C54 C55 1.418(6) . ?
C55 C56 1.367(7) . ?
C55 H55 0.9300 . ?
C56 C57 1.393(7) . ?
C56 H56 0.9300 . ?
C57 N8 1.345(5) . ?
C57 H57 0.9300 . ?
C58 C59 1.395(6) . ?
C58 C63 1.397(6) . ?
C59 C60 1.378(7) . ?
C59 H59 0.9300 . ?
C60 C61 1.383(7) . ?
C60 H60 0.9300 . ?
C61 C62 1.398(7) . ?
C61 S4 1.762(5) . ?
C62 C63 1.370(7) . ?
C62 H62 0.9300 . ?
C63 H63 0.9300 . ?
C64 S4 1.708(19) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C64B S4 1.807(13) . ?
C64B H64D 0.9600 . ?
C64B H64E 0.9600 . ?
C64B H64F 0.9600 . ?
C65 N9 1.345(5) . ?
C65 C66 1.394(7) . ?
C65 H65 0.9300 . ?
C66 C67 1.356(7) . ?
C66 H66 0.9300 . ?
C67 C68 1.419(6) . ?
C67 H67 0.9300 . ?
C68 N9 1.382(5) . ?
C68 C69 1.409(6) . ?
C69 C70 1.412(6) . ?
C69 C74 1.501(6) . ?
C70 N10 1.393(5) . ?
C70 C71 1.417(6) . ?
C71 C72 1.351(6) . ?
C71 H71 0.9300 . ?
C72 C73 1.436(6) . ?
C72 H72 0.9300 . ?
C73 N10 1.352(5) . ?
C73 C81 1.438(6) . ?
C74 C75 1.386(6) . ?
C74 C79 1.388(6) . ?
C75 C76 1.366(6) . ?
C75 H75 0.9300 . ?
C76 C77 1.390(7) . ?
C76 H76 0.9300 . ?
C77 C78 1.371(7) . ?
C77 S5 1.769(5) . ?
C78 C79 1.375(7) . ?
C78 H78 0.9300 . ?
C79 H79 0.9300 . ?
C80 S5 1.95(2) . ?
C80 H80A 0.9600 . ?
C80 H80B 0.9600 . ?
C80 H80C 0.9600 . ?
C80B S5 1.707(13) . ?
C80B H80D 0.9600 . ?
C80B H80E 0.9600 . ?
C80B H80F 0.9600 . ?
C81 N11 1.350(5) . ?
C81 C82 1.420(6) . ?
C82 C83 1.357(6) . ?
C82 H82 0.9300 . ?
C83 C84 1.423(6) . ?
C83 H83 0.9300 . ?
C84 N11 1.406(5) . ?
C84 C85 1.409(6) . ?
C85 C86 1.408(6) . ?
C85 C90 1.489(6) . ?
C86 N12 1.398(6) . ?
C86 C87 1.420(6) . ?
C87 C88 1.369(7) . ?
C87 H87 0.9300 . ?
C88 C89 1.401(7) . ?
C88 H88 0.9300 . ?
C89 N12 1.330(6) . ?
C89 H89 0.9300 . ?
C90 C91 1.394(6) . ?
C90 C95 1.399(6) . ?
C91 C92 1.373(6) . ?
C91 H91 0.9300 . ?
C92 C93 1.395(6) . ?
C92 H92 0.9300 . ?
C93 C94 1.386(6) . ?
C93 S6 1.772(5) . ?
C94 C95 1.372(6) . ?
C94 H94 0.9300 . ?
C95 H95 0.9300 . ?
C96 S6 1.777(6) . ?
C96 H96A 0.9600 . ?
C96 H96B 0.9600 . ?
C96 H96C 0.9600 . ?
N1 Zn1 1.982(3) . ?
N2 Zn1 2.003(3) . ?
N3 Zn3 2.002(3) . ?
N4 Zn3 1.988(3) . ?
N5 Zn1 1.987(3) . ?
N6 Zn1 1.999(3) . ?
N7 Zn2 1.982(3) . ?
N8 Zn2 1.970(3) . ?
N9 Zn2 1.985(4) . ?
N10 Zn2 1.979(3) . ?
N11 Zn3 1.996(3) . ?
N12 Zn3 1.987(3) . ?
C97 C98 1.335(16) . ?
C97 H97A 0.9600 . ?
C97 H97B 0.9600 . ?
C97 H97C 0.9600 . ?
C98 O1 1.249(16) . ?
C98 O2 1.378(16) . ?
C99 C100 1.465(9) . ?
C99 O2 1.516(14) . ?
C99 H99A 0.9700 . ?
C99 H99B 0.9700 . ?
C100 H10A 0.9600 . ?
C100 H10B 0.9600 . ?
C100 H10C 0.9600 . ?
C101 C103 1.361(10) . ?
C101 C103 1.361(10) 2_656 ?
C101 C104 1.371(10) . ?
C101 C104 1.371(10) 2_656 ?
C102 C103 1.358(10) . ?
C102 C104 1.432(10) . ?

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 C1 C2 111.6(4) . . ?
N1 C1 H1 124.2 . . ?
C2 C1 H1 124.2 . . ?
C3 C2 C1 106.9(4) . . ?
C3 C2 H2 126.6 . . ?
C1 C2 H2 126.6 . . ?
C2 C3 C4 107.0(4) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
N1 C4 C5 124.2(4) . . ?
N1 C4 C3 108.3(4) . . ?
C5 C4 C3 127.2(4) . . ?
C4 C5 C6 126.5(4) . . ?
C4 C5 C10 115.6(4) . . ?
C6 C5 C10 118.0(4) . . ?
N2 C6 C5 125.9(4) . . ?
N2 C6 C7 108.0(3) . . ?
C5 C6 C7 126.1(4) . . ?
C8 C7 C6 107.7(4) . . ?
C8 C7 H7 126.2 . . ?
C6 C7 H7 126.2 . . ?
C7 C8 C9 106.6(4) . . ?
C7 C8 H8 126.7 . . ?
C9 C8 H8 126.7 . . ?
N2 C9 C8 110.8(4) . . ?
N2 C9 C17 122.3(4) . . ?
C8 C9 C17 126.9(4) . . ?
C15 C10 C11 117.4(4) . . ?
C15 C10 C5 123.4(4) . . ?
C11 C10 C5 119.2(4) . . ?
C12 C11 C10 122.2(4) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C11 C12 C13 119.7(4) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 118.9(4) . . ?
C14 C13 S1 125.5(4) . . ?
C12 C13 S1 115.6(4) . . ?
C13 C14 C15 120.3(4) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C10 C15 C14 121.5(4) . . ?
C10 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
S1 C16 H16A 109.5 . . ?
S1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
S1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C18 110.4(4) . . ?
N3 C17 C9 123.2(3) . . ?
C18 C17 C9 126.4(4) . . ?
C19 C18 C17 107.1(4) . . ?
C19 C18 H18 126.4 . . ?
C17 C18 H18 126.4 . . ?
C18 C19 C20 107.3(4) . . ?
C18 C19 H19 126.3 . . ?
C20 C19 H19 126.3 . . ?
N3 C20 C21 126.4(3) . . ?
N3 C20 C19 108.5(3) . . ?
C21 C20 C19 125.1(4) . . ?
C22 C21 C20 125.9(4) . . ?
C22 C21 C26 118.0(4) . . ?
C20 C21 C26 116.0(3) . . ?
N4 C22 C21 123.2(4) . . ?
N4 C22 C23 108.0(4) . . ?
C21 C22 C23 128.7(4) . . ?
C24 C23 C22 107.5(4) . . ?
C24 C23 H23 126.3 . . ?
C22 C23 H23 126.3 . . ?
C23 C24 C25 106.2(4) . . ?
C23 C24 H24 126.9 . . ?
C25 C24 H24 126.9 . . ?
N4 C25 C24 111.4(4) . . ?
N4 C25 H25 124.3 . . ?
C24 C25 H25 124.3 . . ?
C27 C26 C31 117.8(4) . . ?
C27 C26 C21 119.8(4) . . ?
C31 C26 C21 122.3(4) . . ?
C28 C27 C26 121.4(4) . . ?
C28 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C27 C28 C29 119.8(4) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C28 119.7(4) . . ?
C30 C29 S2 116.9(3) . . ?
C28 C29 S2 123.4(4) . . ?
C29 C30 C31 121.1(4) . . ?
C29 C30 H30 119.4 . . ?
C31 C30 H30 119.4 . . ?
C30 C31 C26 120.1(4) . . ?
C30 C31 H31 119.9 . . ?
C26 C31 H31 119.9 . . ?
S2 C32 H32A 109.5 . . ?
S2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
S2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N5 C33 C34 111.5(4) . . ?
N5 C33 H33 124.3 . . ?
C34 C33 H33 124.3 . . ?
C35 C34 C33 106.3(4) . . ?
C35 C34 H34 126.9 . . ?
C33 C34 H34 126.9 . . ?
C34 C35 C36 107.4(4) . . ?
C34 C35 H35 126.3 . . ?
C36 C35 H35 126.3 . . ?
N5 C36 C37 123.8(4) . . ?
N5 C36 C35 108.3(4) . . ?
C37 C36 C35 127.9(4) . . ?
C36 C37 C38 126.0(4) . . ?
C36 C37 C42 116.2(3) . . ?
C38 C37 C42 117.9(4) . . ?
N6 C38 C37 125.7(4) . . ?
N6 C38 C39 108.5(3) . . ?
C37 C38 C39 125.7(4) . . ?
C40 C39 C38 107.4(4) . . ?
C40 C39 H39 126.3 . . ?
C38 C39 H39 126.3 . . ?
C39 C40 C41 106.7(4) . . ?
C39 C40 H40 126.6 . . ?
C41 C40 H40 126.6 . . ?
N6 C41 C40 110.7(3) . . ?
N6 C41 C49 121.4(4) . . ?
C40 C41 C49 127.6(4) . . ?
C47 C42 C43 117.8(4) . . ?
C47 C42 C37 120.4(4) . . ?
C43 C42 C37 121.7(4) . . ?
C44 C43 C42 121.0(4) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C43 C44 C45 120.5(4) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C46 C45 C44 118.7(4) . . ?
C46 C45 S3 124.1(4) . . ?
C44 C45 S3 117.1(4) . . ?
C45 C46 C47 120.6(4) . . ?
C45 C46 H46 119.7 . . ?
C47 C46 H46 119.7 . . ?
C46 C47 C42 121.3(4) . . ?
C46 C47 H47 119.3 . . ?
C42 C47 H47 119.3 . . ?
S3 C48 H48A 109.5 . . ?
S3 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
S3 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N7 C49 C50 109.8(3) . . ?
N7 C49 C41 124.4(4) . . ?
C50 C49 C41 125.7(4) . . ?
C51 C50 C49 107.0(4) . . ?
C51 C50 H50 126.5 . . ?
C49 C50 H50 126.5 . . ?
C50 C51 C52 108.0(4) . . ?
C50 C51 H51 126.0 . . ?
C52 C51 H51 126.0 . . ?
N7 C52 C53 127.5(4) . . ?
N7 C52 C51 108.2(3) . . ?
C53 C52 C51 124.2(4) . . ?
C52 C53 C54 126.9(4) . . ?
C52 C53 C58 116.6(4) . . ?
C54 C53 C58 116.3(4) . . ?
N8 C54 C53 122.9(4) . . ?
N8 C54 C55 108.4(4) . . ?
C53 C54 C55 128.4(4) . . ?
C56 C55 C54 107.6(4) . . ?
C56 C55 H55 126.2 . . ?
C54 C55 H55 126.2 . . ?
C55 C56 C57 106.1(4) . . ?
C55 C56 H56 127.0 . . ?
C57 C56 H56 127.0 . . ?
N8 C57 C56 111.7(4) . . ?
N8 C57 H57 124.1 . . ?
C56 C57 H57 124.1 . . ?
C59 C58 C63 117.3(4) . . ?
C59 C58 C53 122.1(4) . . ?
C63 C58 C53 120.6(4) . . ?
C60 C59 C58 121.3(4) . . ?
C60 C59 H59 119.4 . . ?
C58 C59 H59 119.4 . . ?
C59 C60 C61 121.0(4) . . ?
C59 C60 H60 119.5 . . ?
C61 C60 H60 119.5 . . ?
C60 C61 C62 118.1(4) . . ?
C60 C61 S4 117.4(4) . . ?
C62 C61 S4 124.5(4) . . ?
C63 C62 C61 120.9(5) . . ?
C63 C62 H62 119.6 . . ?
C61 C62 H62 119.6 . . ?
C62 C63 C58 121.4(4) . . ?
C62 C63 H63 119.3 . . ?
C58 C63 H63 119.3 . . ?
S4 C64 H64A 109.5 . . ?
S4 C64 H64B 109.5 . . ?
S4 C64 H64C 109.5 . . ?
S4 C64B H64D 109.5 . . ?
S4 C64B H64E 109.5 . . ?
H64D C64B H64E 109.5 . . ?
S4 C64B H64F 109.5 . . ?
H64D C64B H64F 109.5 . . ?
H64E C64B H64F 109.5 . . ?
N9 C65 C66 111.0(4) . . ?
N9 C65 H65 124.5 . . ?
C66 C65 H65 124.5 . . ?
C67 C66 C65 106.8(4) . . ?
C67 C66 H66 126.6 . . ?
C65 C66 H66 126.6 . . ?
C66 C67 C68 107.5(4) . . ?
C66 C67 H67 126.3 . . ?
C68 C67 H67 126.3 . . ?
N9 C68 C69 123.5(4) . . ?
N9 C68 C67 108.2(4) . . ?
C69 C68 C67 128.3(4) . . ?
C68 C69 C70 127.1(4) . . ?
C68 C69 C74 116.1(4) . . ?
C70 C69 C74 116.7(4) . . ?
N10 C70 C69 125.1(4) . . ?
N10 C70 C71 108.5(3) . . ?
C69 C70 C71 126.3(4) . . ?
C72 C71 C70 108.5(4) . . ?
C72 C71 H71 125.8 . . ?
C70 C71 H71 125.8 . . ?
C71 C72 C73 106.2(4) . . ?
C71 C72 H72 126.9 . . ?
C73 C72 H72 126.9 . . ?
N10 C73 C72 110.3(4) . . ?
N10 C73 C81 122.6(4) . . ?
C72 C73 C81 127.0(4) . . ?
C75 C74 C79 117.4(4) . . ?
C75 C74 C69 122.0(4) . . ?
C79 C74 C69 120.6(4) . . ?
C76 C75 C74 121.3(4) . . ?
C76 C75 H75 119.4 . . ?
C74 C75 H75 119.4 . . ?
C75 C76 C77 120.5(4) . . ?
C75 C76 H76 119.7 . . ?
C77 C76 H76 119.7 . . ?
C78 C77 C76 118.9(5) . . ?
C78 C77 S5 124.3(4) . . ?
C76 C77 S5 116.7(4) . . ?
C77 C78 C79 120.2(5) . . ?
C77 C78 H78 119.9 . . ?
C79 C78 H78 119.9 . . ?
C78 C79 C74 121.6(4) . . ?
C78 C79 H79 119.2 . . ?
C74 C79 H79 119.2 . . ?
S5 C80 H80A 109.5 . . ?
S5 C80 H80B 109.5 . . ?
S5 C80 H80C 109.5 . . ?
S5 C80B H80D 109.5 . . ?
S5 C80B H80E 109.5 . . ?
S5 C80B H80F 109.5 . . ?
N11 C81 C82 110.2(4) . . ?
N11 C81 C73 123.0(4) . . ?
C82 C81 C73 126.7(4) . . ?
C83 C82 C81 107.2(4) . . ?
C83 C82 H82 126.4 . . ?
C81 C82 H82 126.4 . . ?
C82 C83 C84 107.8(4) . . ?
C82 C83 H83 126.1 . . ?
C84 C83 H83 126.1 . . ?
N11 C84 C85 126.0(4) . . ?
N11 C84 C83 108.0(4) . . ?
C85 C84 C83 125.5(4) . . ?
C86 C85 C84 126.3(4) . . ?
C86 C85 C90 117.8(4) . . ?
C84 C85 C90 115.9(4) . . ?
N12 C86 C85 123.5(4) . . ?
N12 C86 C87 107.7(4) . . ?
C85 C86 C87 128.7(4) . . ?
C88 C87 C86 107.8(4) . . ?
C88 C87 H87 126.1 . . ?
C86 C87 H87 126.1 . . ?
C87 C88 C89 105.9(4) . . ?
C87 C88 H88 127.1 . . ?
C89 C88 H88 127.1 . . ?
N12 C89 C88 112.0(4) . . ?
N12 C89 H89 124.0 . . ?
C88 C89 H89 124.0 . . ?
C91 C90 C95 117.3(4) . . ?
C91 C90 C85 122.9(4) . . ?
C95 C90 C85 119.8(4) . . ?
C92 C91 C90 121.1(4) . . ?
C92 C91 H91 119.4 . . ?
C90 C91 H91 119.4 . . ?
C91 C92 C93 120.9(4) . . ?
C91 C92 H92 119.5 . . ?
C93 C92 H92 119.5 . . ?
C94 C93 C92 118.5(4) . . ?
C94 C93 S6 116.6(4) . . ?
C92 C93 S6 125.0(4) . . ?
C95 C94 C93 120.4(4) . . ?
C95 C94 H94 119.8 . . ?
C93 C94 H94 119.8 . . ?
C94 C95 C90 121.8(4) . . ?
C94 C95 H95 119.1 . . ?
C90 C95 H95 119.1 . . ?
S6 C96 H96A 109.5 . . ?
S6 C96 H96B 109.5 . . ?
H96A C96 H96B 109.5 . . ?
S6 C96 H96C 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
C1 N1 C4 106.3(4) . . ?
C1 N1 Zn1 129.1(3) . . ?
C4 N1 Zn1 124.6(3) . . ?
C9 N2 C6 106.9(3) . . ?
C9 N2 Zn1 130.2(3) . . ?
C6 N2 Zn1 122.4(3) . . ?
C17 N3 C20 106.6(3) . . ?
C17 N3 Zn3 132.2(3) . . ?
C20 N3 Zn3 121.2(3) . . ?
C25 N4 C22 106.8(3) . . ?
C25 N4 Zn3 124.5(3) . . ?
C22 N4 Zn3 122.0(3) . . ?
C33 N5 C36 106.6(3) . . ?
C33 N5 Zn1 128.2(3) . . ?
C36 N5 Zn1 124.2(3) . . ?
C41 N6 C38 106.7(3) . . ?
C41 N6 Zn1 128.3(3) . . ?
C38 N6 Zn1 119.1(3) . . ?
C49 N7 C52 107.0(3) . . ?
C49 N7 Zn2 132.4(3) . . ?
C52 N7 Zn2 120.5(3) . . ?
C57 N8 C54 106.3(4) . . ?
C57 N8 Zn2 126.2(3) . . ?
C54 N8 Zn2 124.6(3) . . ?
C65 N9 C68 106.5(4) . . ?
C65 N9 Zn2 127.7(3) . . ?
C68 N9 Zn2 125.8(3) . . ?
C73 N10 C70 106.6(3) . . ?
C73 N10 Zn2 129.3(3) . . ?
C70 N10 Zn2 124.0(3) . . ?
C81 N11 C84 106.8(3) . . ?
C81 N11 Zn3 132.2(3) . . ?
C84 N11 Zn3 120.0(3) . . ?
C89 N12 C86 106.6(4) . . ?
C89 N12 Zn3 128.3(3) . . ?
C86 N12 Zn3 122.9(3) . . ?
C13 S1 C16 102.9(3) . . ?
C29 S2 C32 103.9(3) . . ?
C45 S3 C48 103.1(2) . . ?
C64 S4 C61 103.7(6) . . ?
C64 S4 C64B 35.8(8) . . ?
C61 S4 C64B 104.8(4) . . ?
C80B S5 C77 102.9(5) . . ?
C80B S5 C80 38.3(8) . . ?
C77 S5 C80 102.7(6) . . ?
C93 S6 C96 103.0(3) . . ?
N1 Zn1 N5 102.51(14) . . ?
N1 Zn1 N6 127.16(14) . . ?
N5 Zn1 N6 94.72(13) . . ?
N1 Zn1 N2 94.36(14) . . ?
N5 Zn1 N2 124.71(14) . . ?
N6 Zn1 N2 115.68(13) . . ?
N8 Zn2 N10 118.04(14) . . ?
N8 Zn2 N7 96.37(14) . . ?
N10 Zn2 N7 119.99(14) . . ?
N8 Zn2 N9 106.31(14) . . ?
N10 Zn2 N9 94.30(14) . . ?
N7 Zn2 N9 122.75(14) . . ?
N12 Zn3 N4 105.07(14) . . ?
N12 Zn3 N11 93.75(14) . . ?
N4 Zn3 N11 123.23(14) . . ?
N12 Zn3 N3 126.24(14) . . ?
N4 Zn3 N3 93.80(13) . . ?
N11 Zn3 N3 116.96(13) . . ?
C98 C97 H97A 109.5 . . ?
C98 C97 H97B 109.5 . . ?
H97A C97 H97B 109.5 . . ?
C98 C97 H97C 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
O1 C98 C97 122.8(18) . . ?
O1 C98 O2 96.7(13) . . ?
C97 C98 O2 140.5(18) . . ?
C100 C99 O2 101.0(11) . . ?
C100 C99 H99A 111.6 . . ?
O2 C99 H99A 111.6 . . ?
C100 C99 H99B 111.6 . . ?
O2 C99 H99B 111.6 . . ?
H99A C99 H99B 109.4 . . ?
C99 C100 H10A 109.5 . . ?
C99 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
C99 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C98 O2 C99 114.0(12) . . ?
C103 C101 C103 180.0(12) . 2_656 ?
C103 C101 C104 73.4(11) . . ?
C103 C101 C104 106.6(11) 2_656 . ?
C103 C101 C104 106.6(11) . 2_656 ?
C103 C101 C104 73.4(11) 2_656 2_656 ?
C104 C101 C104 180.0(17) . 2_656 ?
C103 C102 C104 71.5(11) . . ?
C102 C103 C101 109.2(12) . . ?
C101 C104 C102 104.5(11) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        29.43
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         1.371
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.129
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound1b
_database_code_depnum_ccdc_archive 'CCDC 1040040'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H26 N4 Ni O4'

_chemical_formula_sum            'C34 H26 N4 Ni O4'
_chemical_formula_weight         613.30

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   9.2124(3)
_cell_length_b                   11.1476(3)
_cell_length_c                   14.7168(5)
_cell_angle_alpha                86.1660(10)
_cell_angle_beta                 76.5000(10)
_cell_angle_gamma                70.6820(10)
_cell_volume                     1386.77(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9887
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      28.90

_exptl_crystal_description       prism
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8961
_exptl_absorpt_correction_T_max  0.9495
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26775
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         29.07
_reflns_number_total             7382
_reflns_number_gt                6081
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0522P)²+0.9963P] 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         7382
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1089
_refine_ls_wR_factor_gt          0.1010
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
C1 C 1.0083(2) 0.3234(2) 0.68500(14) 0.0292(4) Uani 1 1 d . . .
H1 H 1.0666 0.3758 0.6898 0.035 Uiso 1 1 calc R . .
C2 C 1.0733(2) 0.1926(2) 0.66784(15) 0.0312(5) Uani 1 1 d . . .
H2 H 1.1793 0.1439 0.6595 0.037 Uiso 1 1 calc R . .
C3 C 0.9507(2) 0.1500(2) 0.66567(14) 0.0274(4) Uani 1 1 d . . .
H3 H 0.9579 0.0668 0.6550 0.033 Uiso 1 1 calc R . .
C4 C 0.8111(2) 0.25628(18) 0.68265(12) 0.0210(4) Uani 1 1 d . . .
C5 C 0.6549(2) 0.25772(18) 0.69598(12) 0.0207(4) Uani 1 1 d . . .
C6 C 0.5252(2) 0.36309(19) 0.73065(13) 0.0228(4) Uani 1 1 d . . .
C7 C 0.3630(2) 0.3826(2) 0.73457(16) 0.0303(4) Uani 1 1 d . . .
H7 H 0.3216 0.3235 0.7184 0.036 Uiso 1 1 calc R . .
C8 C 0.2795(3) 0.5035(2) 0.76643(18) 0.0357(5) Uani 1 1 d . . .
H8 H 0.1710 0.5430 0.7755 0.043 Uiso 1 1 calc R . .
C9 C 0.3901(2) 0.5570(2) 0.78284(15) 0.0288(4) Uani 1 1 d . . .
H9 H 0.3643 0.6394 0.8049 0.035 Uiso 1 1 calc R . .
C10 C 0.6250(2) 0.14115(19) 0.67278(13) 0.0235(4) Uani 1 1 d . . .
C11 C 0.6963(3) 0.0791(2) 0.58736(15) 0.0295(4) Uani 1 1 d . . .
H11 H 0.7669 0.1088 0.5436 0.035 Uiso 1 1 calc R . .
C12 C 0.6623(3) -0.0281(2) 0.56684(16) 0.0339(5) Uani 1 1 d . . .
H12 H 0.7109 -0.0703 0.5098 0.041 Uiso 1 1 calc R . .
C13 C 0.5555(3) -0.0714(2) 0.63203(17) 0.0334(5) Uani 1 1 d . . .
C14 C 0.4861(3) -0.0111(2) 0.71697(17) 0.0353(5) Uani 1 1 d . . .
H14 H 0.4160 -0.0413 0.7607 0.042 Uiso 1 1 calc R . .
C15 C 0.5198(2) 0.0945(2) 0.73803(15) 0.0298(4) Uani 1 1 d . . .
H15 H 0.4723 0.1347 0.7959 0.036 Uiso 1 1 calc R . .
C16 C 0.5057(3) -0.1815(2) 0.61340(18) 0.0401(5) Uani 1 1 d . . .
C17 C 0.5617(5) -0.3616(3) 0.5221(2) 0.0631(9) Uani 1 1 d . . .
H17A H 0.5738 -0.4191 0.5734 0.095 Uiso 1 1 calc R . .
H17B H 0.6310 -0.4033 0.4656 0.095 Uiso 1 1 calc R . .
H17C H 0.4545 -0.3355 0.5154 0.095 Uiso 1 1 calc R . .
C18 C 0.5448(2) 0.61364(19) 0.93275(13) 0.0255(4) Uani 1 1 d . . .
H18 H 0.4830 0.5615 0.9364 0.031 Uiso 1 1 calc R . .
C19 C 0.5521(2) 0.6775(2) 1.00969(14) 0.0275(4) Uani 1 1 d . . .
H19 H 0.4993 0.6743 1.0715 0.033 Uiso 1 1 calc R . .
C20 C 0.6528(2) 0.74573(19) 0.97564(13) 0.0245(4) Uani 1 1 d . . .
H20 H 0.6800 0.7988 1.0100 0.029 Uiso 1 1 calc R . .
C21 C 0.7077(2) 0.71980(18) 0.87792(12) 0.0210(4) Uani 1 1 d . . .
C22 C 0.8207(2) 0.76143(18) 0.81565(13) 0.0202(4) Uani 1 1 d . . .
C23 C 0.8891(2) 0.71155(18) 0.72493(13) 0.0212(4) Uani 1 1 d . . .
C24 C 0.9840(2) 0.7568(2) 0.64930(14) 0.0275(4) Uani 1 1 d . . .
H24 H 1.0216 0.8241 0.6514 0.033 Uiso 1 1 calc R . .
C25 C 1.0098(3) 0.6829(2) 0.57269(14) 0.0340(5) Uani 1 1 d . . .
H25 H 1.0673 0.6906 0.5129 0.041 Uiso 1 1 calc R . .
C26 C 0.9321(3) 0.5931(2) 0.60252(14) 0.0336(5) Uani 1 1 d . . .
H26 H 0.9305 0.5309 0.5640 0.040 Uiso 1 1 calc R . .
C27 C 0.8707(2) 0.86378(18) 0.84605(12) 0.0208(4) Uani 1 1 d . . .
C28 C 0.7599(2) 0.97431(19) 0.88798(13) 0.0245(4) Uani 1 1 d . . .
H28 H 0.6532 0.9828 0.9010 0.029 Uiso 1 1 calc R . .
C29 C 0.8067(2) 1.07262(19) 0.91077(14) 0.0257(4) Uani 1 1 d . . .
H29 H 0.7314 1.1471 0.9380 0.031 Uiso 1 1 calc R . .
C30 C 0.9658(2) 1.05971(18) 0.89291(13) 0.0236(4) Uani 1 1 d . . .
C31 C 1.0773(2) 0.9470(2) 0.85503(14) 0.0276(4) Uani 1 1 d . . .
H31 H 1.1842 0.9365 0.8456 0.033 Uiso 1 1 calc R . .
C32 C 1.0303(2) 0.84999(19) 0.83120(14) 0.0262(4) Uani 1 1 d . . .
H32 H 1.1058 0.7750 0.8051 0.031 Uiso 1 1 calc R . .
C33 C 1.0218(3) 1.1657(2) 0.90953(13) 0.0266(4) Uani 1 1 d . . .
C34 C 0.9459(3) 1.3800(2) 0.95617(19) 0.0434(6) Uani 1 1 d . . .
H34A H 1.0047 1.3606 1.0043 0.065 Uiso 1 1 calc R . .
H34B H 0.8525 1.4517 0.9753 0.065 Uiso 1 1 calc R . .
H34C H 1.0098 1.3997 0.8995 0.065 Uiso 1 1 calc R . .
N1 N 0.85076(19) 0.36439(16) 0.69369(11) 0.0230(3) Uani 1 1 d . . .
N2 N 0.53636(19) 0.47467(15) 0.76268(11) 0.0224(3) Uani 1 1 d . . .
N3 N 0.63743(19) 0.63669(16) 0.85327(11) 0.0222(3) Uani 1 1 d . . .
N4 N 0.8607(2) 0.60821(16) 0.69349(11) 0.0250(3) Uani 1 1 d . . .
O1 O 0.3926(3) -0.2032(2) 0.65871(17) 0.0671(6) Uani 1 1 d . . .
O2 O 0.6014(2) -0.24981(17) 0.53998(13) 0.0491(5) Uani 1 1 d . . .
O3 O 1.15878(19) 1.15776(16) 0.89578(12) 0.0383(4) Uani 1 1 d . . .
O4 O 0.90211(19) 1.27172(14) 0.94024(12) 0.0354(4) Uani 1 1 d . . .
Ni1 Ni 0.71907(3) 0.52214(2) 0.750167(16) 0.02081(8) Uani 1 1 d . . .


_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
C1 N1 1.347(3) . ?
C1 C2 1.396(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.370(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.414(3) . ?
C3 H3 0.9300 . ?
C4 N1 1.399(2) . ?
C4 C5 1.401(3) . ?
C5 C6 1.391(3) . ?
C5 C10 1.490(2) . ?
C6 N2 1.402(2) . ?
C6 C7 1.425(3) . ?
C7 C8 1.364(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.410(3) . ?
C8 H8 0.9300 . ?
C9 N2 1.333(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.386(3) . ?
C10 C15 1.402(3) . ?
C11 C12 1.399(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.390(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(3) . ?
C13 C16 1.506(3) . ?
C14 C15 1.383(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.187(3) . ?
C16 O2 1.321(3) . ?
C17 O2 1.465(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N3 1.342(2) . ?
C18 C19 1.403(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.374(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.424(2) . ?
C20 H20 0.9300 . ?
C21 C22 1.399(2) . ?
C21 N3 1.400(2) . ?
C22 C23 1.401(3) . ?
C22 C27 1.492(2) . ?
C23 N4 1.392(2) . ?
C23 C24 1.421(3) . ?
C24 C25 1.369(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.406(3) . ?
C25 H25 0.9300 . ?
C26 N4 1.341(2) . ?
C26 H26 0.9300 . ?
C27 C28 1.384(3) . ?
C27 C32 1.391(3) . ?
C28 C29 1.389(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.387(3) . ?
C29 H29 0.9300 . ?
C30 C31 1.384(3) . ?
C30 C33 1.491(3) . ?
C31 C32 1.383(3) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 O3 1.204(3) . ?
C33 O4 1.339(3) . ?
C34 O4 1.442(2) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
N1 Ni1 1.8890(17) . ?
N2 Ni1 1.8917(15) . ?
N3 Ni1 1.8946(15) . ?
N4 Ni1 1.8790(16) . ?

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 C1 C2 111.64(17) . . ?
N1 C1 H1 124.2 . . ?
C2 C1 H1 124.2 . . ?
C3 C2 C1 106.63(19) . . ?
C3 C2 H2 126.7 . . ?
C1 C2 H2 126.7 . . ?
C2 C3 C4 107.28(18) . . ?
C2 C3 H3 126.4 . . ?
C4 C3 H3 126.4 . . ?
N1 C4 C5 123.03(18) . . ?
N1 C4 C3 108.68(16) . . ?
C5 C4 C3 128.04(18) . . ?
C6 C5 C4 123.05(17) . . ?
C6 C5 C10 118.03(16) . . ?
C4 C5 C10 118.91(18) . . ?
C5 C6 N2 123.87(17) . . ?
C5 C6 C7 128.04(17) . . ?
N2 C6 C7 107.96(17) . . ?
C8 C7 C6 107.53(18) . . ?
C8 C7 H7 126.2 . . ?
C6 C7 H7 126.2 . . ?
C7 C8 C9 106.47(19) . . ?
C7 C8 H8 126.8 . . ?
C9 C8 H8 126.8 . . ?
N2 C9 C8 111.51(19) . . ?
N2 C9 H9 124.2 . . ?
C8 C9 H9 124.2 . . ?
C11 C10 C15 119.06(18) . . ?
C11 C10 C5 121.60(17) . . ?
C15 C10 C5 119.33(18) . . ?
C10 C11 C12 120.11(19) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 120.25(19) . . ?
C14 C13 C16 116.6(2) . . ?
C12 C13 C16 123.1(2) . . ?
C13 C14 C15 120.3(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C10 120.4(2) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
O1 C16 O2 124.1(2) . . ?
O1 C16 C13 123.9(2) . . ?
O2 C16 C13 112.0(2) . . ?
O2 C17 H17A 109.5 . . ?
O2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 112.00(17) . . ?
N3 C18 H18 124.0 . . ?
C19 C18 H18 124.0 . . ?
C20 C19 C18 106.37(17) . . ?
C20 C19 H19 126.8 . . ?
C18 C19 H19 126.8 . . ?
C19 C20 C21 107.05(16) . . ?
C19 C20 H20 126.5 . . ?
C21 C20 H20 126.5 . . ?
C22 C21 N3 123.96(16) . . ?
C22 C21 C20 127.17(16) . . ?
N3 C21 C20 108.74(15) . . ?
C21 C22 C23 122.73(16) . . ?
C21 C22 C27 119.17(16) . . ?
C23 C22 C27 118.10(16) . . ?
N4 C23 C22 122.06(16) . . ?
N4 C23 C24 108.51(16) . . ?
C22 C23 C24 129.28(17) . . ?
C25 C24 C23 107.36(17) . . ?
C25 C24 H24 126.3 . . ?
C23 C24 H24 126.3 . . ?
C24 C25 C26 106.27(17) . . ?
C24 C25 H25 126.9 . . ?
C26 C25 H25 126.9 . . ?
N4 C26 C25 111.54(18) . . ?
N4 C26 H26 124.2 . . ?
C25 C26 H26 124.2 . . ?
C28 C27 C32 119.02(17) . . ?
C28 C27 C22 120.79(16) . . ?
C32 C27 C22 120.19(17) . . ?
C27 C28 C29 120.56(18) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C30 C29 C28 119.99(18) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C31 C30 C29 119.60(17) . . ?
C31 C30 C33 118.23(18) . . ?
C29 C30 C33 122.12(18) . . ?
C32 C31 C30 120.23(18) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C27 120.49(19) . . ?
C31 C32 H32 119.8 . . ?
C27 C32 H32 119.8 . . ?
O3 C33 O4 123.75(18) . . ?
O3 C33 C30 124.1(2) . . ?
O4 C33 C30 112.20(17) . . ?
O4 C34 H34A 109.5 . . ?
O4 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O4 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C1 N1 C4 105.76(17) . . ?
C1 N1 Ni1 122.44(13) . . ?
C4 N1 Ni1 128.65(13) . . ?
C9 N2 C6 106.52(16) . . ?
C9 N2 Ni1 123.39(13) . . ?
C6 N2 Ni1 128.14(13) . . ?
C18 N3 C21 105.82(15) . . ?
C18 N3 Ni1 122.28(13) . . ?
C21 N3 Ni1 126.57(12) . . ?
C26 N4 C23 106.30(16) . . ?
C26 N4 Ni1 122.05(13) . . ?
C23 N4 Ni1 130.44(13) . . ?
C16 O2 C17 113.8(2) . . ?
C33 O4 C34 115.84(18) . . ?
N4 Ni1 N1 93.72(7) . . ?
N4 Ni1 N2 153.98(7) . . ?
N1 Ni1 N2 91.78(7) . . ?
N4 Ni1 N3 91.20(7) . . ?
N1 Ni1 N3 151.43(7) . . ?
N2 Ni1 N3 96.03(7) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        29.07
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.067
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound2b
_database_code_depnum_ccdc_archive 'CCDC 1040041'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H24 N4 Ni O4'
_chemical_formula_sum            'C34 H24 N4 Ni O4'
_chemical_formula_weight         611.28

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'
Ni Ni 0.3393 1.1124 '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                   34.4732(8)
_cell_length_b                   9.8680(2)
_cell_length_c                   7.9143(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.7240(10)
_cell_angle_gamma                90.00
_cell_volume                     2645.28(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9963
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      29.98

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9187
_exptl_absorpt_correction_T_max  0.9187
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28830
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         29.59
_reflns_number_total             3688
_reflns_number_gt                3289
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0500P)²+2.5665P] 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         3688
_refine_ls_number_parameters     196
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.1003
_refine_ls_wR_factor_gt          0.0879
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.141
_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
C1 C 0.46080(5) 0.05580(17) 0.1180(2) 0.0244(3) Uani 1 1 d . . .
H1 H 0.4846 0.0140 0.1107 0.029 Uiso 1 1 calc R . .
C2 C 0.42357(5) -0.00360(18) 0.0611(2) 0.0269(3) Uani 1 1 d . . .
H2 H 0.4185 -0.0887 0.0113 0.032 Uiso 1 1 calc R . .
C3 C 0.39620(4) 0.08982(17) 0.0941(2) 0.0239(3) Uani 1 1 d . . .
H3 H 0.3689 0.0790 0.0722 0.029 Uiso 1 1 calc R . .
C4 C 0.41745(4) 0.20624(16) 0.16812(19) 0.0207(3) Uani 1 1 d . . .
C5 C 0.40122(4) 0.33350(17) 0.19569(19) 0.0214(3) Uani 1 1 d . . .
C6 C 0.42418(4) 0.45096(17) 0.2239(2) 0.0246(3) Uani 1 1 d . . .
C7 C 0.41426(5) 0.59024(18) 0.2457(2) 0.0290(3) Uani 1 1 d . . .
H7 H 0.3893 0.6237 0.2513 0.035 Uiso 1 1 calc R . .
C8 C 0.44831(5) 0.66553(19) 0.2571(3) 0.0318(4) Uani 1 1 d . . .
H8 H 0.4508 0.7589 0.2705 0.038 Uiso 1 1 calc R . .
C9 C 0.47881(5) 0.57205(17) 0.2441(2) 0.0280(3) Uani 1 1 d . . .
C10 C 0.35769(4) 0.34316(16) 0.18478(18) 0.0207(3) Uani 1 1 d . . .
C11 C 0.33834(4) 0.25438(17) 0.27976(19) 0.0218(3) Uani 1 1 d . . .
H11 H 0.3528 0.1887 0.3486 0.026 Uiso 1 1 calc R . .
C12 C 0.29780(4) 0.26319(16) 0.27255(18) 0.0210(3) Uani 1 1 d . . .
H12 H 0.2853 0.2037 0.3363 0.025 Uiso 1 1 calc R . .
C13 C 0.27596(4) 0.36152(16) 0.16942(18) 0.0196(3) Uani 1 1 d . . .
C14 C 0.29478(4) 0.44877(17) 0.07240(19) 0.0235(3) Uani 1 1 d . . .
H14 H 0.2802 0.5136 0.0025 0.028 Uiso 1 1 calc R . .
C15 C 0.33528(4) 0.43958(17) 0.0793(2) 0.0239(3) Uani 1 1 d . . .
H15 H 0.3476 0.4979 0.0135 0.029 Uiso 1 1 calc R . .
C16 C 0.23263(4) 0.37729(16) 0.16051(18) 0.0209(3) Uani 1 1 d . . .
C17 C 0.17768(5) 0.31016(19) 0.2760(2) 0.0287(4) Uani 1 1 d . . .
H17A H 0.1713 0.4030 0.2944 0.043 Uiso 1 1 calc R . .
H17B H 0.1711 0.2552 0.3666 0.043 Uiso 1 1 calc R . .
H17C H 0.1629 0.2801 0.1675 0.043 Uiso 1 1 calc R . .
N1 N 0.45794(4) 0.17988(13) 0.18405(17) 0.0213(3) Uani 1 1 d . . .
N2 N 0.46413(4) 0.44504(14) 0.22544(19) 0.0259(3) Uani 1 1 d . . .
O1 O 0.21187(3) 0.45292(13) 0.06312(16) 0.0296(3) Uani 1 1 d . . .
O2 O 0.21932(3) 0.29848(12) 0.27511(15) 0.0262(2) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.30375(3) 0.2500 0.02109(9) Uani 1 2 d S . .


_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
C1 N1 1.342(2) . ?
C1 C2 1.406(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.378(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.428(2) . ?
C3 H3 0.9300 . ?
C4 N1 1.4022(18) . ?
C4 C5 1.408(2) . ?
C5 C6 1.398(2) . ?
C5 C10 1.490(2) . ?
C6 N2 1.3765(18) . ?
C6 C7 1.435(2) . ?
C7 C8 1.378(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.417(2) . ?
C8 H8 0.9300 . ?
C9 N2 1.349(2) . ?
C9 C9 1.446(3) 2_655 ?
C10 C15 1.400(2) . ?
C10 C11 1.402(2) . ?
C11 C12 1.391(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.395(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.392(2) . ?
C13 C16 1.4905(19) . ?
C14 C15 1.390(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.2073(19) . ?
C16 O2 1.3389(19) . ?
C17 O2 1.4413(18) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
N1 Ni1 1.8940(13) . ?
N2 Ni1 1.8496(14) . ?
Ni1 N2 1.8496(14) 2_655 ?
Ni1 N1 1.8940(13) 2_655 ?

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 C1 C2 112.10(14) . . ?
N1 C1 H1 123.9 . . ?
C2 C1 H1 123.9 . . ?
C3 C2 C1 106.06(15) . . ?
C3 C2 H2 127.0 . . ?
C1 C2 H2 127.0 . . ?
C2 C3 C4 107.37(13) . . ?
C2 C3 H3 126.3 . . ?
C4 C3 H3 126.3 . . ?
N1 C4 C5 124.69(14) . . ?
N1 C4 C3 108.28(13) . . ?
C5 C4 C3 126.33(14) . . ?
C6 C5 C4 122.31(13) . . ?
C6 C5 C10 119.37(14) . . ?
C4 C5 C10 118.23(14) . . ?
N2 C6 C5 120.15(14) . . ?
N2 C6 C7 107.46(14) . . ?
C5 C6 C7 132.31(14) . . ?
C8 C7 C6 107.77(14) . . ?
C8 C7 H7 126.1 . . ?
C6 C7 H7 126.1 . . ?
C7 C8 C9 106.20(16) . . ?
C7 C8 H8 126.9 . . ?
C9 C8 H8 126.9 . . ?
N2 C9 C8 110.15(14) . . ?
N2 C9 C9 111.14(9) . 2_655 ?
C8 C9 C9 138.56(11) . 2_655 ?
C15 C10 C11 118.66(13) . . ?
C15 C10 C5 121.09(14) . . ?
C11 C10 C5 120.25(13) . . ?
C12 C11 C10 120.93(14) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 119.76(14) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 119.79(13) . . ?
C14 C13 C16 118.38(13) . . ?
C12 C13 C16 121.83(13) . . ?
C15 C14 C13 120.39(14) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C10 120.46(14) . . ?
C14 C15 H15 119.8 . . ?
C10 C15 H15 119.8 . . ?
O1 C16 O2 123.67(14) . . ?
O1 C16 C13 124.36(14) . . ?
O2 C16 C13 111.96(12) . . ?
O2 C17 H17A 109.5 . . ?
O2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1 N1 C4 106.15(13) . . ?
C1 N1 Ni1 126.03(10) . . ?
C4 N1 Ni1 127.10(10) . . ?
C9 N2 C6 108.41(13) . . ?
C9 N2 Ni1 117.32(11) . . ?
C6 N2 Ni1 132.94(12) . . ?
C16 O2 C17 115.07(12) . . ?
N2 Ni1 N2 82.15(8) 2_655 . ?
N2 Ni1 N1 89.72(6) 2_655 2_655 ?
N2 Ni1 N1 167.95(6) . 2_655 ?
N2 Ni1 N1 167.95(6) 2_655 . ?
N2 Ni1 N1 89.72(6) . . ?
N1 Ni1 N1 99.61(8) 2_655 . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        29.59
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.072
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound3b
_database_code_depnum_ccdc_archive 'CCDC 1040042'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H26 N4 O4'
_chemical_formula_sum            'C34 H26 N4 O4'
_chemical_formula_weight         554.59

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2/c  '

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

_cell_length_a                   20.8248(7)
_cell_length_b                   7.2192(2)
_cell_length_c                   19.4469(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.8250(10)
_cell_angle_gamma                90.00
_cell_volume                     2812.81(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7590
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      24.98

_exptl_crystal_description       rod
_exptl_crystal_colour            dark-purple
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9913
_exptl_absorpt_correction_T_max  0.9974
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41843
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         29.74
_reflns_number_total             7843
_reflns_number_gt                4731
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0574P)²+1.4266P] 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         7843
_refine_ls_number_parameters     391
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1538
_refine_ls_wR_factor_gt          0.1259
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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
C1 C 0.62813(11) 0.2927(4) 1.06097(12) 0.0518(6) Uani 1 1 d . . .
H1A H 0.6300 0.2089 1.0978 0.062 Uiso 1 1 calc R . .
C2 C 0.58121(10) 0.4304(4) 1.03923(13) 0.0532(6) Uani 1 1 d . . .
H2 H 0.5460 0.4561 1.0586 0.064 Uiso 1 1 calc R . .
C3 C 0.59614(10) 0.5237(3) 0.98309(12) 0.0460(5) Uani 1 1 d . . .
H3A H 0.5726 0.6231 0.9579 0.055 Uiso 1 1 calc R . .
C4 C 0.65278(9) 0.4413(3) 0.97138(10) 0.0373(4) Uani 1 1 d . . .
C5 C 0.68988(9) 0.4888(3) 0.92223(9) 0.0330(4) Uani 1 1 d . . .
C6 C 0.74751(9) 0.3989(3) 0.91882(9) 0.0326(4) Uani 1 1 d . . .
C7 C 0.79164(10) 0.4386(3) 0.87495(10) 0.0385(5) Uani 1 1 d . . .
H7 H 0.7876 0.5361 0.8428 0.046 Uiso 1 1 calc R . .
C8 C 0.83995(10) 0.3081(3) 0.88926(10) 0.0384(5) Uani 1 1 d . . .
H8 H 0.8757 0.2986 0.8694 0.046 Uiso 1 1 calc R . .
C9 C 0.82496(9) 0.1864(3) 0.94166(9) 0.0318(4) Uani 1 1 d . . .
C10 C 0.85961(9) 0.0214(3) 0.97255(9) 0.0311(4) Uani 1 1 d . . .
C11 C 0.91812(9) -0.0617(3) 0.96540(9) 0.0354(4) Uani 1 1 d . . .
H11 H 0.9445 -0.0201 0.9369 0.042 Uiso 1 1 calc R . .
C12 C 0.92942(10) -0.2180(3) 1.00868(9) 0.0348(4) Uani 1 1 d . . .
H12 H 0.9648 -0.3003 1.0144 0.042 Uiso 1 1 calc R . .
C13 C 0.87782(9) -0.2294(3) 1.04219(9) 0.0298(4) Uani 1 1 d . . .
C14 C 0.86533(8) -0.3595(2) 1.09244(9) 0.0289(4) Uani 1 1 d . . .
C15 C 0.80817(9) -0.3571(3) 1.11554(9) 0.0311(4) Uani 1 1 d . . .
C16 C 0.79272(9) -0.4661(3) 1.17100(10) 0.0368(4) Uani 1 1 d . . .
H16 H 0.8192 -0.5584 1.1980 0.044 Uiso 1 1 calc R . .
C17 C 0.73231(10) -0.4086(3) 1.17639(11) 0.0440(5) Uani 1 1 d . . .
H17 H 0.7092 -0.4534 1.2076 0.053 Uiso 1 1 calc R . .
C18 C 0.71131(10) -0.2654(3) 1.12438(11) 0.0423(5) Uani 1 1 d . . .
H18 H 0.6710 -0.2025 1.1168 0.051 Uiso 1 1 calc R . .
C19 C 0.66181(9) 0.6374(3) 0.86882(10) 0.0339(4) Uani 1 1 d . . .
C20 C 0.61672(14) 0.5889(3) 0.80566(13) 0.0659(8) Uani 1 1 d . . .
H20 H 0.6050 0.4650 0.7970 0.079 Uiso 1 1 calc R . .
C21 C 0.58834(13) 0.7198(3) 0.75468(13) 0.0603(7) Uani 1 1 d . . .
H21 H 0.5578 0.6832 0.7124 0.072 Uiso 1 1 calc R . .
C22 C 0.60478(10) 0.9026(3) 0.76583(11) 0.0389(5) Uani 1 1 d . A .
C23 C 0.65104(15) 0.9516(3) 0.82801(15) 0.0778(10) Uani 1 1 d . . .
H23 H 0.6639 1.0749 0.8358 0.093 Uiso 1 1 calc R . .
C24 C 0.67890(15) 0.8204(3) 0.87946(15) 0.0765(10) Uani 1 1 d . . .
H24 H 0.7095 0.8570 0.9217 0.092 Uiso 1 1 calc R . .
C25 C 0.57376(12) 1.0467(3) 0.71221(13) 0.0521(6) Uani 1 1 d . . .
C26 C 0.49682(16) 1.1112(4) 0.60217(16) 0.0861(10) Uani 1 1 d . . .
H26A H 0.4766 1.2041 0.6248 0.129 Uiso 1 1 calc R A .
H26B H 0.4629 1.0489 0.5662 0.129 Uiso 1 1 calc R . .
H26C H 0.5280 1.1687 0.5805 0.129 Uiso 1 1 calc R . .
C27 C 0.91911(9) -0.4977(2) 1.12147(9) 0.0283(4) Uani 1 1 d . . .
C28 C 0.98386(9) -0.4378(3) 1.15301(9) 0.0309(4) Uani 1 1 d . . .
H28 H 0.9931 -0.3116 1.1566 0.037 Uiso 1 1 calc R . .
C29 C 1.03476(9) -0.5639(2) 1.17907(9) 0.0295(4) Uani 1 1 d . . .
H29 H 1.0779 -0.5220 1.2001 0.035 Uiso 1 1 calc R . .
C30 C 1.02160(9) -0.7528(2) 1.17392(8) 0.0276(4) Uani 1 1 d . . .
C31 C 0.95668(9) -0.8136(3) 1.14308(9) 0.0304(4) Uani 1 1 d . . .
H31 H 0.9475 -0.9398 1.1398 0.037 Uiso 1 1 calc R . .
C32 C 0.90588(9) -0.6877(3) 1.11725(9) 0.0303(4) Uani 1 1 d . . .
H32 H 0.8626 -0.7297 1.0969 0.036 Uiso 1 1 calc R . .
C33 C 1.07466(9) -0.8931(3) 1.20184(9) 0.0309(4) Uani 1 1 d . . .
C34 C 1.18918(11) -0.9454(3) 1.25530(14) 0.0592(7) Uani 1 1 d . . .
H34A H 1.1795 -1.0119 1.2941 0.089 Uiso 1 1 calc R . .
H34B H 1.2301 -0.8779 1.2727 0.089 Uiso 1 1 calc R . .
H34C H 1.1936 -1.0314 1.2192 0.089 Uiso 1 1 calc R . .
N1 N 0.67080(8) 0.2997(3) 1.01999(9) 0.0441(4) Uani 1 1 d . . .
H1 H 0.7042 0.2267 1.0237 0.053 Uiso 1 1 calc R . .
N2 N 0.77100(7) 0.2417(2) 0.95987(8) 0.0318(3) Uani 1 1 d . . .
N3 N 0.83627(7) -0.0818(2) 1.01846(7) 0.0303(3) Uani 1 1 d . . .
H3 H 0.8006 -0.0583 1.0310 0.036 Uiso 1 1 calc R . .
N4 N 0.75532(7) -0.2320(2) 1.08839(8) 0.0362(4) Uani 1 1 d . . .
O1A O 0.5968(7) 1.2059(9) 0.7136(3) 0.065(2) Uani 0.58(4) 1 d P A 1
O1B O 0.564(2) 1.2028(13) 0.7298(13) 0.103(10) Uani 0.42(4) 1 d P A 2
O2 O 0.53142(9) 0.9786(2) 0.65496(9) 0.0659(5) Uani 1 1 d . A .
O3 O 1.06498(7) -1.05763(19) 1.20311(8) 0.0420(3) Uani 1 1 d . . .
O4 O 1.13542(6) -0.81751(18) 1.22513(7) 0.0394(3) Uani 1 1 d . . .


_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
C1 N1 1.347(3) . ?
C1 C2 1.377(3) . ?
C1 H1A 0.9300 . ?
C2 C3 1.388(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(3) . ?
C3 H3A 0.9300 . ?
C4 N1 1.374(3) . ?
C4 C5 1.425(3) . ?
C5 C6 1.382(3) . ?
C5 C19 1.497(3) . ?
C6 N2 1.397(2) . ?
C6 C7 1.443(3) . ?
C7 C8 1.351(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.442(3) . ?
C8 H8 0.9300 . ?
C9 N2 1.328(2) . ?
C9 C10 1.437(3) . ?
C10 N3 1.351(2) . ?
C10 C11 1.399(3) . ?
C11 C12 1.389(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.403(3) . ?
C12 H12 0.9300 . ?
C13 N3 1.371(2) . ?
C13 C14 1.429(3) . ?
C14 C15 1.382(3) . ?
C14 C27 1.491(2) . ?
C15 N4 1.410(2) . ?
C15 C16 1.441(3) . ?
C16 C17 1.355(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.429(3) . ?
C17 H17 0.9300 . ?
C18 N4 1.318(3) . ?
C18 H18 0.9300 . ?
C19 C24 1.369(3) . ?
C19 C20 1.373(3) . ?
C20 C21 1.380(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.366(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.371(3) . ?
C22 C25 1.490(3) . ?
C23 C24 1.385(3) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O1B 1.210(15) . ?
C25 O1A 1.243(7) . ?
C25 O2 1.313(3) . ?
C26 O2 1.444(3) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.389(2) . ?
C27 C32 1.397(3) . ?
C28 C29 1.384(2) . ?
C28 H28 0.9300 . ?
C29 C30 1.389(3) . ?
C29 H29 0.9300 . ?
C30 C31 1.392(2) . ?
C30 C33 1.488(2) . ?
C31 C32 1.381(2) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 O3 1.206(2) . ?
C33 O4 1.339(2) . ?
C34 O4 1.446(2) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
N1 H1 0.8600 . ?
N3 H3 0.8600 . ?

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 C1 C2 108.6(2) . . ?
N1 C1 H1A 125.7 . . ?
C2 C1 H1A 125.7 . . ?
C1 C2 C3 107.4(2) . . ?
C1 C2 H2 126.3 . . ?
C3 C2 H2 126.3 . . ?
C2 C3 C4 107.6(2) . . ?
C2 C3 H3A 126.2 . . ?
C4 C3 H3A 126.2 . . ?
N1 C4 C3 106.83(19) . . ?
N1 C4 C5 122.97(17) . . ?
C3 C4 C5 130.1(2) . . ?
C6 C5 C4 123.80(17) . . ?
C6 C5 C19 118.90(17) . . ?
C4 C5 C19 117.20(17) . . ?
C5 C6 N2 121.83(17) . . ?
C5 C6 C7 129.55(17) . . ?
N2 C6 C7 108.60(16) . . ?
C8 C7 C6 107.35(17) . . ?
C8 C7 H7 126.3 . . ?
C6 C7 H7 126.3 . . ?
C7 C8 C9 106.14(17) . . ?
C7 C8 H8 126.9 . . ?
C9 C8 H8 126.9 . . ?
N2 C9 C10 120.15(16) . . ?
N2 C9 C8 111.55(16) . . ?
C10 C9 C8 128.28(17) . . ?
N3 C10 C11 108.01(16) . . ?
N3 C10 C9 120.22(16) . . ?
C11 C10 C9 131.76(18) . . ?
C12 C11 C10 107.25(17) . . ?
C12 C11 H11 126.4 . . ?
C10 C11 H11 126.4 . . ?
C11 C12 C13 107.73(16) . . ?
C11 C12 H12 126.1 . . ?
C13 C12 H12 126.1 . . ?
N3 C13 C12 106.92(16) . . ?
N3 C13 C14 121.68(16) . . ?
C12 C13 C14 131.40(16) . . ?
C15 C14 C13 123.18(16) . . ?
C15 C14 C27 120.64(16) . . ?
C13 C14 C27 116.14(16) . . ?
C14 C15 N4 122.66(17) . . ?
C14 C15 C16 128.65(17) . . ?
N4 C15 C16 108.62(16) . . ?
C17 C16 C15 106.99(18) . . ?
C17 C16 H16 126.5 . . ?
C15 C16 H16 126.5 . . ?
C16 C17 C18 106.15(19) . . ?
C16 C17 H17 126.9 . . ?
C18 C17 H17 126.9 . . ?
N4 C18 C17 112.66(18) . . ?
N4 C18 H18 123.7 . . ?
C17 C18 H18 123.7 . . ?
C24 C19 C20 117.88(19) . . ?
C24 C19 C5 123.40(17) . . ?
C20 C19 C5 118.72(18) . . ?
C19 C20 C21 121.5(2) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C22 C21 C20 120.5(2) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 118.3(2) . . ?
C21 C22 C25 121.42(19) . . ?
C23 C22 C25 120.2(2) . . ?
C22 C23 C24 121.0(2) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C19 C24 C23 120.7(2) . . ?
C19 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
O1B C25 O1A 39.2(18) . . ?
O1B C25 O2 117.7(7) . . ?
O1A C25 O2 122.1(4) . . ?
O1B C25 C22 121.7(9) . . ?
O1A C25 C22 122.6(5) . . ?
O2 C25 C22 113.3(2) . . ?
O2 C26 H26A 109.5 . . ?
O2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C32 118.91(16) . . ?
C28 C27 C14 119.83(16) . . ?
C32 C27 C14 121.26(16) . . ?
C29 C28 C27 120.76(17) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 120.18(16) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C29 C30 C31 119.34(16) . . ?
C29 C30 C33 121.99(16) . . ?
C31 C30 C33 118.66(16) . . ?
C32 C31 C30 120.45(17) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C31 C32 C27 120.36(16) . . ?
C31 C32 H32 119.8 . . ?
C27 C32 H32 119.8 . . ?
O3 C33 O4 122.85(17) . . ?
O3 C33 C30 124.50(17) . . ?
O4 C33 C30 112.65(16) . . ?
O4 C34 H34A 109.5 . . ?
O4 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O4 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C1 N1 C4 109.55(18) . . ?
C1 N1 H1 125.2 . . ?
C4 N1 H1 125.2 . . ?
C9 N2 C6 106.34(15) . . ?
C10 N3 C13 110.08(15) . . ?
C10 N3 H3 125.0 . . ?
C13 N3 H3 125.0 . . ?
C18 N4 C15 105.58(16) . . ?
C25 O2 C26 116.4(2) . . ?
C33 O4 C34 115.64(16) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        29.74
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.046
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound4b
_database_code_depnum_ccdc_archive 'CCDC 1040043'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H48 N8 O8 Zn2'
_chemical_formula_sum            'C68 H48 N8 O8 Zn2'
_chemical_formula_weight         1235.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           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                   23.8065(15)
_cell_length_b                   16.6644(11)
_cell_length_c                   42.744(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.563(2)
_cell_angle_gamma                90.00
_cell_volume                     16670.1(18)
_cell_formula_units_Z            12
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8151
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      23.46

_exptl_crystal_description       block
_exptl_crystal_colour            dark-green
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7632
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9126
_exptl_absorpt_correction_T_max  0.9292
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
For two phenyl rings, two carbon atoms are disordered over
 two positions. The PART command has been used to model 
this positional disorder.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            110709
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_theta_min         1.50
_diffrn_reflns_theta_max         29.42
_reflns_number_total             22429
_reflns_number_gt                13288
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0787P)²+93.0417P] 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         22429
_refine_ls_number_parameters     1206
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.0775
_refine_ls_wR_factor_ref         0.2190
_refine_ls_wR_factor_gt          0.1884
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_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
C1 C 0.3531(2) -0.1030(3) 0.26502(12) 0.0321(11) Uani 1 1 d . . .
H1 H 0.3407 -0.0584 0.2749 0.039 Uiso 1 1 calc R . .
C2 C 0.3362(2) -0.1834(3) 0.26968(13) 0.0388(12) Uani 1 1 d . . .
H2 H 0.3109 -0.2001 0.2826 0.047 Uiso 1 1 calc R . .
C3 C 0.3639(2) -0.2309(3) 0.25168(13) 0.0342(11) Uani 1 1 d . . .
H3 H 0.3616 -0.2866 0.2501 0.041 Uiso 1 1 calc R . .
C4 C 0.39726(19) -0.1793(2) 0.23546(11) 0.0246(9) Uani 1 1 d . . .
C5 C 0.43222(19) -0.2003(2) 0.21408(11) 0.0249(9) Uani 1 1 d . . .
C6 C 0.46812(19) -0.1497(2) 0.20031(11) 0.0239(9) Uani 1 1 d . . .
C7 C 0.4950(2) -0.1660(3) 0.17382(12) 0.0326(11) Uani 1 1 d . . .
H7 H 0.4941 -0.2143 0.1629 0.039 Uiso 1 1 calc R . .
C8 C 0.5224(2) -0.0975(3) 0.16749(12) 0.0338(11) Uani 1 1 d . . .
H8 H 0.5427 -0.0900 0.1511 0.041 Uiso 1 1 calc R . .
C9 C 0.5140(2) -0.0404(2) 0.19049(11) 0.0263(10) Uani 1 1 d . . .
C10 C 0.4307(2) -0.2869(3) 0.20406(12) 0.0301(10) Uani 1 1 d . . .
C11 C 0.4813(2) -0.3309(2) 0.20863(13) 0.0351(12) Uani 1 1 d . . .
H11 H 0.5157 -0.3058 0.2169 0.042 Uiso 1 1 calc R . .
C12 C 0.4808(2) -0.4121(3) 0.20100(15) 0.0441(14) Uani 1 1 d . . .
H12 H 0.5146 -0.4415 0.2045 0.053 Uiso 1 1 calc R . .
C13 C 0.4289(2) -0.4490(3) 0.18793(15) 0.0460(15) Uani 1 1 d . . .
C14 C 0.3790(2) -0.4048(3) 0.18296(14) 0.0437(14) Uani 1 1 d . . .
H14 H 0.3447 -0.4290 0.1739 0.052 Uiso 1 1 calc R . .
C15 C 0.3800(2) -0.3245(3) 0.19139(13) 0.0381(12) Uani 1 1 d . . .
H15 H 0.3461 -0.2956 0.1885 0.046 Uiso 1 1 calc R . .
C16 C 0.4254(3) -0.5362(4) 0.17909(18) 0.0620(19) Uani 1 1 d . . .
C17 C 0.4748(4) -0.6567(3) 0.1749(2) 0.097(3) Uani 1 1 d . . .
H17A H 0.4540 -0.6868 0.1882 0.146 Uiso 1 1 calc R . .
H17B H 0.5132 -0.6766 0.1775 0.146 Uiso 1 1 calc R . .
H17C H 0.4565 -0.6623 0.1531 0.146 Uiso 1 1 calc R . .
C18 C 0.53976(19) 0.0380(2) 0.19710(11) 0.0262(10) Uani 1 1 d . . .
C19 C 0.5517(2) 0.0976(3) 0.17565(12) 0.0352(12) Uani 1 1 d . . .
H19 H 0.5454 0.0942 0.1536 0.042 Uiso 1 1 calc R . .
C20 C 0.5743(2) 0.1614(3) 0.19403(13) 0.0357(12) Uani 1 1 d . . .
H20 H 0.5859 0.2100 0.1866 0.043 Uiso 1 1 calc R . .
C21 C 0.5770(2) 0.1398(2) 0.22641(12) 0.0281(10) Uani 1 1 d . . .
C22 C 0.60114(19) 0.1846(2) 0.25339(13) 0.0294(11) Uani 1 1 d . A .
C23 C 0.61083(19) 0.1593(2) 0.28477(12) 0.0289(10) Uani 1 1 d . . .
C24 C 0.6313(2) 0.2058(3) 0.31255(13) 0.0406(13) Uani 1 1 d . . .
H24 H 0.6426 0.2592 0.3130 0.049 Uiso 1 1 calc R . .
C25 C 0.6313(3) 0.1577(3) 0.33804(15) 0.0486(15) Uani 1 1 d . . .
H25 H 0.6419 0.1719 0.3593 0.058 Uiso 1 1 calc R . .
C26 C 0.6119(2) 0.0810(3) 0.32589(14) 0.0403(13) Uani 1 1 d . . .
H26 H 0.6083 0.0363 0.3384 0.048 Uiso 1 1 calc R . .
C27 C 0.6184(2) 0.2700(2) 0.24780(12) 0.0307(11) Uani 1 1 d . . .
C28 C 0.5806(3) 0.3292(3) 0.2449(2) 0.067(2) Uani 1 1 d . A .
H28 H 0.5425 0.3169 0.2449 0.080 Uiso 1 1 calc R . .
C29 C 0.5959(3) 0.4089(3) 0.2421(2) 0.069(2) Uani 1 1 d . . .
H29 H 0.5683 0.4489 0.2409 0.082 Uiso 1 1 calc R A .
C30 C 0.6497(2) 0.4284(2) 0.24090(12) 0.0308(11) Uani 1 1 d . A .
C32A C 0.6896(5) 0.3736(6) 0.2524(7) 0.045(5) Uani 0.50(3) 1 d P A 1
H32A H 0.7277 0.3888 0.2576 0.054 Uiso 0.50(3) 1 calc PR A 1
C33A C 0.6742(6) 0.2939(6) 0.2568(7) 0.046(6) Uani 0.50(3) 1 d P A 1
H33A H 0.7018 0.2571 0.2658 0.055 Uiso 0.50(3) 1 calc PR A 1
C32B C 0.6857(6) 0.3646(8) 0.2325(6) 0.041(5) Uani 0.50(3) 1 d P A 2
H32B H 0.7192 0.3762 0.2251 0.049 Uiso 0.50(3) 1 calc PR A 2
C33B C 0.6689(6) 0.2871(7) 0.2358(7) 0.038(5) Uani 0.50(3) 1 d P A 2
H33B H 0.6908 0.2452 0.2300 0.045 Uiso 0.50(3) 1 calc PR A 2
C33 C 0.6647(2) 0.5146(2) 0.23757(12) 0.0318(11) Uani 1 1 d . . .
C34 C 0.7391(3) 0.6075(3) 0.23744(19) 0.064(2) Uani 1 1 d . . .
H34A H 0.7166 0.6330 0.2192 0.096 Uiso 1 1 calc R A .
H34B H 0.7786 0.6081 0.2354 0.096 Uiso 1 1 calc R . .
H34C H 0.7347 0.6359 0.2564 0.096 Uiso 1 1 calc R . .
N1 N 0.38913(16) -0.10045(19) 0.24469(9) 0.0252(8) Uani 1 1 d . . .
N2 N 0.48112(16) -0.07072(19) 0.21014(9) 0.0231(8) Uani 1 1 d . . .
N3 N 0.55443(16) 0.06320(19) 0.22732(9) 0.0242(8) Uani 1 1 d . . .
N4 N 0.59954(17) 0.0816(2) 0.29455(10) 0.0287(9) Uani 1 1 d . . .
O1 O 0.3818(2) -0.5702(3) 0.16939(19) 0.109(2) Uani 1 1 d . . .
O2 O 0.4758(2) -0.5721(2) 0.18396(13) 0.0666(14) Uani 1 1 d . . .
O3 O 0.63115(18) 0.5682(2) 0.23348(12) 0.0589(12) Uani 1 1 d . A .
O4 O 0.72042(17) 0.5256(2) 0.23942(12) 0.0581(12) Uani 1 1 d . A .
Zn1 Zn 0.43284(2) -0.00651(3) 0.234156(13) 0.02461(13) Uani 1 1 d . . .
C35 C 0.3028(2) 0.1959(3) 0.07794(12) 0.0367(12) Uani 1 1 d . . .
H35 H 0.3180 0.1561 0.0667 0.044 Uiso 1 1 calc R . .
C36 C 0.3200(2) 0.2766(3) 0.07936(14) 0.0420(13) Uani 1 1 d . . .
H36 H 0.3483 0.2990 0.0697 0.050 Uiso 1 1 calc R . .
C37 C 0.2876(2) 0.3156(3) 0.09741(13) 0.0387(12) Uani 1 1 d . . .
H37 H 0.2894 0.3700 0.1023 0.046 Uiso 1 1 calc R . .
C38 C 0.2505(2) 0.2586(3) 0.10743(12) 0.0309(11) Uani 1 1 d . . .
C39 C 0.2083(2) 0.2727(3) 0.12553(12) 0.0310(11) Uani 1 1 d . . .
C40 C 0.1694(2) 0.2163(3) 0.13321(12) 0.0309(11) Uani 1 1 d . . .
C41 C 0.1321(2) 0.2274(3) 0.15554(13) 0.0402(13) Uani 1 1 d . . .
H41 H 0.1271 0.2746 0.1663 0.048 Uiso 1 1 calc R . .
C42 C 0.1049(2) 0.1558(3) 0.15808(13) 0.0375(12) Uani 1 1 d . . .
H42 H 0.0790 0.1445 0.1713 0.045 Uiso 1 1 calc R . .
C43 C 0.1241(2) 0.1025(3) 0.13661(12) 0.0319(11) Uani 1 1 d . . .
C44 C 0.2040(2) 0.3566(3) 0.13714(13) 0.0362(12) Uani 1 1 d . . .
C45 C 0.2451(3) 0.3873(3) 0.16143(15) 0.0489(15) Uani 1 1 d . . .
H45 H 0.2742 0.3544 0.1717 0.059 Uiso 1 1 calc R . .
C46 C 0.2425(3) 0.4680(3) 0.17043(16) 0.0494(15) Uani 1 1 d . . .
H46 H 0.2691 0.4882 0.1873 0.059 Uiso 1 1 calc R . .
C47 C 0.2004(2) 0.5173(3) 0.15415(15) 0.0447(14) Uani 1 1 d . . .
C48 C 0.1583(2) 0.4863(3) 0.13051(14) 0.0428(13) Uani 1 1 d . . .
H48 H 0.1295 0.5194 0.1199 0.051 Uiso 1 1 calc R . .
C49 C 0.1594(2) 0.4057(3) 0.12282(13) 0.0398(12) Uani 1 1 d . . .
H49 H 0.1299 0.3841 0.1079 0.048 Uiso 1 1 calc R . .
C50 C 0.2047(3) 0.6054(3) 0.16152(18) 0.0521(16) Uani 1 1 d . . .
C51 C 0.1764(4) 0.7341(4) 0.1462(2) 0.080(2) Uani 1 1 d . . .
H51A H 0.1770 0.7464 0.1682 0.120 Uiso 1 1 calc R . .
H51B H 0.1455 0.7623 0.1332 0.120 Uiso 1 1 calc R . .
H51C H 0.2119 0.7505 0.1405 0.120 Uiso 1 1 calc R . .
C52 C 0.1026(2) 0.0236(3) 0.12712(12) 0.0312(11) Uani 1 1 d . . .
C53 C 0.0878(2) -0.0407(3) 0.14541(14) 0.0410(13) Uani 1 1 d . . .
H53 H 0.0892 -0.0414 0.1673 0.049 Uiso 1 1 calc R . .
C54 C 0.0708(2) -0.1023(3) 0.12425(13) 0.0414(13) Uani 1 1 d . . .
H54 H 0.0593 -0.1532 0.1294 0.050 Uiso 1 1 calc R . .
C55 C 0.0740(2) -0.0749(3) 0.09343(12) 0.0322(11) Uani 1 1 d . . .
C56 C 0.0577(2) -0.1160(3) 0.06497(13) 0.0350(12) Uani 1 1 d . B .
C57 C 0.0573(2) -0.0870(3) 0.03425(13) 0.0389(12) Uani 1 1 d . . .
C58 C 0.0455(3) -0.1298(4) 0.00479(16) 0.0548(16) Uani 1 1 d . . .
H58 H 0.0330 -0.1826 0.0020 0.066 Uiso 1 1 calc R . .
C59 C 0.0561(3) -0.0781(4) -0.01875(15) 0.0586(18) Uani 1 1 d . . .
H59 H 0.0537 -0.0899 -0.0402 0.070 Uiso 1 1 calc R . .
C60 C 0.0711(3) -0.0045(3) -0.00375(14) 0.0470(14) Uani 1 1 d . . .
H60 H 0.0794 0.0417 -0.0143 0.056 Uiso 1 1 calc R . .
C61 C 0.0375(2) -0.2007(3) 0.06745(14) 0.0382(12) Uani 1 1 d . . .
C62A C -0.0131(11) -0.2158(11) 0.0784(6) 0.044(6) Uani 0.47(5) 1 d P B 3
H62A H -0.0357 -0.1721 0.0814 0.053 Uiso 0.47(5) 1 calc PR B 3
C63A C -0.0325(10) -0.2930(11) 0.0851(8) 0.048(6) Uani 0.47(5) 1 d P B 3
H63A H -0.0650 -0.3012 0.0939 0.058 Uiso 0.47(5) 1 calc PR B 3
C62B C -0.0210(10) -0.2159(12) 0.0593(17) 0.110(18) Uani 0.53(5) 1 d P B 4
H62B H -0.0472 -0.1783 0.0494 0.132 Uiso 0.53(5) 1 calc PR B 4
C63B C -0.0366(7) -0.2943(10) 0.0673(12) 0.064(9) Uani 0.53(5) 1 d P B 4
H63B H -0.0753 -0.3051 0.0657 0.076 Uiso 0.53(5) 1 calc PR B 4
C64 C 0.0017(2) -0.3561(3) 0.07749(14) 0.0404(13) Uani 1 1 d . . .
C65 C 0.0551(2) -0.3426(3) 0.07212(18) 0.0587(19) Uani 1 1 d . B .
H65 H 0.0796 -0.3856 0.0712 0.070 Uiso 1 1 calc R . .
C66 C 0.0736(2) -0.2650(3) 0.06794(18) 0.0572(18) Uani 1 1 d . B .
H66 H 0.1111 -0.2565 0.0654 0.069 Uiso 1 1 calc R . .
C67 C -0.0164(3) -0.4405(3) 0.08294(15) 0.0458(14) Uani 1 1 d . B .
C68 C -0.0921(3) -0.5240(4) 0.0904(2) 0.074(2) Uani 1 1 d . B .
H68A H -0.0875 -0.5594 0.0734 0.111 Uiso 1 1 calc R . .
H68B H -0.1320 -0.5201 0.0916 0.111 Uiso 1 1 calc R . .
H68C H -0.0714 -0.5447 0.1102 0.111 Uiso 1 1 calc R . .
C69 C 0.2605(3) 0.0094(3) 0.16484(15) 0.0494(15) Uani 1 1 d . . .
H69 H 0.2533 0.0566 0.1750 0.059 Uiso 1 1 calc R . .
C70 C 0.2796(3) -0.0627(3) 0.18082(14) 0.0503(15) Uani 1 1 d . . .
H70 H 0.2857 -0.0720 0.2026 0.060 Uiso 1 1 calc R . .
C71 C 0.2872(3) -0.1156(3) 0.15772(14) 0.0455(14) Uani 1 1 d . . .
H71 H 0.3012 -0.1677 0.1609 0.055 Uiso 1 1 calc R . .
C72 C 0.2698(2) -0.0767(3) 0.12774(13) 0.0360(11) Uani 1 1 d . . .
C73 C 0.2671(2) -0.1099(3) 0.09732(13) 0.0357(12) Uani 1 1 d . . .
C74 C 0.2460(2) -0.0704(3) 0.06841(13) 0.0347(11) Uani 1 1 d . . .
C75 C 0.2500(2) -0.0972(3) 0.03722(13) 0.0413(13) Uani 1 1 d . . .
H75 H 0.2639 -0.1466 0.0321 0.050 Uiso 1 1 calc R . .
C76 C 0.2296(2) -0.0376(3) 0.01612(13) 0.0400(13) Uani 1 1 d . . .
H76 H 0.2273 -0.0382 -0.0058 0.048 Uiso 1 1 calc R . .
C77 C 0.2131(2) 0.0249(3) 0.03466(12) 0.0340(11) Uani 1 1 d . . .
C78 C 0.2886(2) -0.1929(3) 0.09576(14) 0.0402(13) Uani 1 1 d . . .
C79 C 0.2534(3) -0.2515(3) 0.07937(16) 0.0503(15) Uani 1 1 d . . .
H79 H 0.2164 -0.2384 0.0696 0.060 Uiso 1 1 calc R . .
C80 C 0.2732(3) -0.3302(3) 0.07741(16) 0.0562(17) Uani 1 1 d . . .
H80 H 0.2491 -0.3693 0.0668 0.067 Uiso 1 1 calc R . .
C81 C 0.3286(3) -0.3497(3) 0.09126(16) 0.0502(15) Uani 1 1 d . . .
C82 C 0.3635(3) -0.2920(3) 0.10783(15) 0.0496(15) Uani 1 1 d . . .
H82 H 0.4005 -0.3056 0.1175 0.060 Uiso 1 1 calc R . .
C83 C 0.3442(2) -0.2132(3) 0.11030(15) 0.0459(14) Uani 1 1 d . . .
H83 H 0.3681 -0.1748 0.1215 0.055 Uiso 1 1 calc R . .
C84 C 0.3472(3) -0.4341(4) 0.08742(18) 0.0608(18) Uani 1 1 d . . .
C85 C 0.4254(4) -0.5219(5) 0.0979(2) 0.097(3) Uani 1 1 d . . .
H85A H 0.4045 -0.5606 0.1078 0.145 Uiso 1 1 calc R . .
H85B H 0.4648 -0.5225 0.1082 0.145 Uiso 1 1 calc R . .
H85C H 0.4228 -0.5351 0.0758 0.145 Uiso 1 1 calc R . .
C86 C 0.1889(2) 0.1030(3) 0.02433(12) 0.0326(11) Uani 1 1 d . . .
C87 C 0.2023(2) 0.1532(3) 0.00070(13) 0.0410(13) Uani 1 1 d . . .
H87 H 0.2257 0.1409 -0.0138 0.049 Uiso 1 1 calc R . .
C88 C 0.1742(2) 0.2246(3) 0.00306(13) 0.0402(13) Uani 1 1 d . . .
H88 H 0.1762 0.2707 -0.0090 0.048 Uiso 1 1 calc R . .
C89 C 0.1412(2) 0.2141(3) 0.02760(11) 0.0301(10) Uani 1 1 d . . .
C90 C 0.1034(2) 0.2697(3) 0.03736(12) 0.0331(11) Uani 1 1 d . . .
C91 C 0.0640(2) 0.2551(3) 0.05687(12) 0.0336(11) Uani 1 1 d . . .
C92 C 0.0321(2) 0.3123(3) 0.07091(13) 0.0400(13) Uani 1 1 d . . .
H92 H 0.0320 0.3676 0.0680 0.048 Uiso 1 1 calc R . .
C93 C 0.0016(2) 0.2707(3) 0.08954(14) 0.0437(13) Uani 1 1 d . . .
H93 H -0.0232 0.2922 0.1018 0.052 Uiso 1 1 calc R . .
C94 C 0.0148(2) 0.1887(3) 0.08674(14) 0.0419(13) Uani 1 1 d . . .
H94 H -0.0002 0.1473 0.0973 0.050 Uiso 1 1 calc R . .
C95 C 0.1107(2) 0.3549(3) 0.02757(12) 0.0339(11) Uani 1 1 d . . .
C96 C 0.1610(2) 0.3952(3) 0.03949(13) 0.0388(12) Uani 1 1 d . . .
H96 H 0.1907 0.3678 0.0523 0.047 Uiso 1 1 calc R . .
C97 C 0.1677(2) 0.4750(3) 0.03278(14) 0.0433(13) Uani 1 1 d . . .
H97 H 0.2012 0.5015 0.0417 0.052 Uiso 1 1 calc R . .
C98 C 0.1249(3) 0.5160(3) 0.01297(14) 0.0456(14) Uani 1 1 d . . .
C99 C 0.0750(3) 0.4764(3) 0.00036(16) 0.0547(17) Uani 1 1 d . . .
H99 H 0.0465 0.5034 -0.0134 0.066 Uiso 1 1 calc R . .
C100 C 0.0668(3) 0.3970(3) 0.00801(14) 0.0460(14) Uani 1 1 d . . .
H100 H 0.0323 0.3716 0.0002 0.055 Uiso 1 1 calc R . .
C101 C 0.1342(4) 0.6031(3) 0.00658(15) 0.0556(18) Uani 1 1 d . . .
C102 C 0.1160(5) 0.7143(5) -0.0242(3) 0.118(4) Uani 1 1 d . . .
H10A H 0.1438 0.7347 -0.0069 0.176 Uiso 1 1 calc R . .
H10B H 0.0831 0.7488 -0.0276 0.176 Uiso 1 1 calc R . .
H10C H 0.1324 0.7127 -0.0431 0.176 Uiso 1 1 calc R . .
N5 N 0.26163(17) 0.1836(2) 0.09478(10) 0.0316(9) Uani 1 1 d . . .
N6 N 0.16310(17) 0.1380(2) 0.12185(9) 0.0295(9) Uani 1 1 d . . .
N7 N 0.09455(17) 0.0035(2) 0.09582(10) 0.0306(9) Uani 1 1 d . . .
N8 N 0.0721(2) -0.0086(2) 0.02750(11) 0.0408(11) Uani 1 1 d . . .
N9 N 0.25427(18) 0.0015(2) 0.13364(10) 0.0343(9) Uani 1 1 d . . .
N10 N 0.22207(18) 0.0058(2) 0.06560(10) 0.0326(9) Uani 1 1 d . . .
N11 N 0.15092(18) 0.1373(2) 0.04020(10) 0.0309(9) Uani 1 1 d . . .
N12 N 0.05161(18) 0.1784(2) 0.06701(10) 0.0340(9) Uani 1 1 d . . .
O5 O 0.2372(2) 0.6327(3) 0.18368(14) 0.0792(16) Uani 1 1 d . . .
O6 O 0.16886(19) 0.6488(2) 0.14123(11) 0.0546(11) Uani 1 1 d . . .
O7 O 0.0153(2) -0.4956(2) 0.08631(13) 0.0674(14) Uani 1 1 d . . .
O8 O -0.0707(2) -0.4463(2) 0.08474(14) 0.0726(15) Uani 1 1 d . . .
O9 O 0.3188(3) -0.4861(3) 0.07386(14) 0.0869(18) Uani 1 1 d . . .
O10 O 0.4022(2) -0.4443(2) 0.10064(13) 0.0696(14) Uani 1 1 d . . .
O11 O 0.1727(2) 0.6411(3) 0.02065(14) 0.0748(15) Uani 1 1 d . . .
O12 O 0.0987(3) 0.6321(3) -0.01650(13) 0.0890(19) Uani 1 1 d . . .
Zn2 Zn 0.22139(2) 0.08264(3) 0.101314(14) 0.03113(15) Uani 1 1 d . . .
Zn3 Zn 0.09289(2) 0.07858(3) 0.059471(14) 0.03076(15) Uani 1 1 d . . .


_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
C1 N1 1.329(6) . ?
C1 C2 1.423(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.357(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.434(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(6) . ?
C4 N1 1.395(5) . ?
C5 C6 1.405(6) . ?
C5 C10 1.503(6) . ?
C6 N2 1.399(5) . ?
C6 C7 1.425(6) . ?
C7 C8 1.365(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.409(6) . ?
C8 H8 0.9300 . ?
C9 N2 1.347(5) . ?
C9 C18 1.448(6) . ?
C10 C15 1.380(7) . ?
C10 C11 1.392(7) . ?
C11 C12 1.391(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.402(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.380(8) . ?
C13 C16 1.500(7) . ?
C14 C15 1.385(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.188(8) . ?
C16 O2 1.323(8) . ?
C17 O2 1.462(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N3 1.342(6) . ?
C18 C19 1.415(6) . ?
C19 C20 1.372(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.421(7) . ?
C20 H20 0.9300 . ?
C21 N3 1.388(5) . ?
C21 C22 1.405(7) . ?
C22 C23 1.385(7) . ?
C22 C27 1.512(6) . ?
C23 N4 1.400(5) . ?
C23 C24 1.427(7) . ?
C24 C25 1.353(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.425(7) . ?
C25 H25 0.9300 . ?
C26 N4 1.318(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.327(7) . ?
C27 C33A 1.372(14) . ?
C27 C33B 1.421(14) . ?
C28 C29 1.388(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.332(7) . ?
C29 H29 0.9300 . ?
C30 C32A 1.344(15) . ?
C30 C32B 1.451(16) . ?
C30 C33 1.493(6) . ?
C32A C33A 1.399(14) . ?
C32A H32A 0.9300 . ?
C33A H33A 0.9300 . ?
C32B C33B 1.367(16) . ?
C32B H32B 0.9300 . ?
C33B H33B 0.9300 . ?
C33 O3 1.188(6) . ?
C33 O4 1.328(6) . ?
C34 O4 1.444(6) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
N1 Zn1 1.977(3) . ?
N2 Zn1 1.988(3) . ?
N3 Zn1 1.993(4) 2_655 ?
N4 Zn1 1.978(4) 2_655 ?
Zn1 N4 1.978(4) 2_655 ?
Zn1 N3 1.993(4) 2_655 ?
C35 N5 1.333(6) . ?
C35 C36 1.405(7) . ?
C35 H35 0.9300 . ?
C36 C37 1.353(8) . ?
C36 H36 0.9300 . ?
C37 C38 1.415(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.395(7) . ?
C38 N5 1.407(6) . ?
C39 C40 1.401(6) . ?
C39 C44 1.493(6) . ?
C40 N6 1.389(6) . ?
C40 C41 1.431(7) . ?
C41 C42 1.371(7) . ?
C41 H41 0.9300 . ?
C42 C43 1.412(7) . ?
C42 H42 0.9300 . ?
C43 N6 1.352(6) . ?
C43 C52 1.441(6) . ?
C44 C45 1.386(8) . ?
C44 C49 1.391(7) . ?
C45 C46 1.403(7) . ?
C45 H45 0.9300 . ?
C46 C47 1.383(8) . ?
C46 H46 0.9300 . ?
C47 C48 1.386(8) . ?
C47 C50 1.501(7) . ?
C48 C49 1.385(7) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
C50 O5 1.197(8) . ?
C50 O6 1.316(8) . ?
C51 O6 1.445(7) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 N7 1.358(6) . ?
C52 C53 1.408(6) . ?
C53 C54 1.379(8) . ?
C53 H53 0.9300 . ?
C54 C55 1.409(7) . ?
C54 H54 0.9300 . ?
C55 C56 1.388(7) . ?
C55 N7 1.392(5) . ?
C56 C57 1.397(8) . ?
C56 C61 1.501(6) . ?
C57 N8 1.396(6) . ?
C57 C58 1.430(8) . ?
C58 C59 1.383(9) . ?
C58 H58 0.9300 . ?
C59 C60 1.401(8) . ?
C59 H59 0.9300 . ?
C60 N8 1.334(7) . ?
C60 H60 0.9300 . ?
C61 C66 1.371(7) . ?
C61 C62A 1.39(2) . ?
C61 C62B 1.40(3) . ?
C62A C63A 1.41(3) . ?
C62A H62A 0.9300 . ?
C63A C64 1.404(18) . ?
C63A H63A 0.9300 . ?
C62B C63B 1.42(3) . ?
C62B H62B 0.9300 . ?
C63B C64 1.39(2) . ?
C63B H63B 0.9300 . ?
C64 C65 1.351(8) . ?
C64 C67 1.500(7) . ?
C65 C66 1.388(7) . ?
C65 H65 0.9300 . ?
C66 H66 0.9300 . ?
C67 O7 1.180(7) . ?
C67 O8 1.313(7) . ?
C68 O8 1.429(7) . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C69 N9 1.321(7) . ?
C69 C70 1.415(8) . ?
C69 H69 0.9300 . ?
C70 C71 1.360(8) . ?
C70 H70 0.9300 . ?
C71 C72 1.428(8) . ?
C71 H71 0.9300 . ?
C72 N9 1.389(6) . ?
C72 C73 1.404(7) . ?
C73 C74 1.409(7) . ?
C73 C78 1.480(6) . ?
C74 N10 1.388(6) . ?
C74 C75 1.425(7) . ?
C75 C76 1.369(7) . ?
C75 H75 0.9300 . ?
C76 C77 1.408(7) . ?
C76 H76 0.9300 . ?
C77 N10 1.339(6) . ?
C77 C86 1.458(6) . ?
C78 C79 1.390(8) . ?
C78 C83 1.396(8) . ?
C79 C80 1.402(8) . ?
C79 H79 0.9300 . ?
C80 C81 1.381(9) . ?
C80 H80 0.9300 . ?
C81 C82 1.378(8) . ?
C81 C84 1.492(8) . ?
C82 C83 1.402(7) . ?
C82 H82 0.9300 . ?
C83 H83 0.9300 . ?
C84 O9 1.184(8) . ?
C84 O10 1.337(8) . ?
C85 O10 1.420(7) . ?
C85 H85A 0.9600 . ?
C85 H85B 0.9600 . ?
C85 H85C 0.9600 . ?
C86 N11 1.353(6) . ?
C86 C87 1.393(7) . ?
C87 C88 1.378(7) . ?
C87 H87 0.9300 . ?
C88 C89 1.431(7) . ?
C88 H88 0.9300 . ?
C89 N11 1.391(6) . ?
C89 C90 1.409(7) . ?
C90 C91 1.386(7) . ?
C90 C95 1.499(6) . ?
C91 N12 1.398(6) . ?
C91 C92 1.419(7) . ?
C92 C93 1.362(8) . ?
C92 H92 0.9300 . ?
C93 C94 1.412(7) . ?
C93 H93 0.9300 . ?
C94 N12 1.334(6) . ?
C94 H94 0.9300 . ?
C95 C96 1.385(7) . ?
C95 C100 1.400(7) . ?
C96 C97 1.377(7) . ?
C96 H96 0.9300 . ?
C97 C98 1.379(8) . ?
C97 H97 0.9300 . ?
C98 C99 1.378(9) . ?
C98 C101 1.501(7) . ?
C99 C100 1.387(7) . ?
C99 H99 0.9300 . ?
C100 H100 0.9300 . ?
C101 O11 1.183(8) . ?
C101 O12 1.271(8) . ?
C102 O12 1.486(9) . ?
C102 H10A 0.9600 . ?
C102 H10B 0.9600 . ?
C102 H10C 0.9600 . ?
N5 Zn2 1.981(4) . ?
N6 Zn2 1.999(4) . ?
N7 Zn3 1.990(4) . ?
N8 Zn3 1.994(4) . ?
N9 Zn2 1.989(4) . ?
N10 Zn2 1.994(4) . ?
N11 Zn3 1.990(4) . ?
N12 Zn3 1.988(4) . ?

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 C1 C2 110.8(4) . . ?
N1 C1 H1 124.6 . . ?
C2 C1 H1 124.6 . . ?
C3 C2 C1 106.9(4) . . ?
C3 C2 H2 126.6 . . ?
C1 C2 H2 126.6 . . ?
C2 C3 C4 107.1(4) . . ?
C2 C3 H3 126.5 . . ?
C4 C3 H3 126.5 . . ?
C5 C4 N1 123.7(4) . . ?
C5 C4 C3 128.2(4) . . ?
N1 C4 C3 108.1(4) . . ?
C4 C5 C6 127.4(4) . . ?
C4 C5 C10 116.4(4) . . ?
C6 C5 C10 116.2(4) . . ?
N2 C6 C5 123.9(4) . . ?
N2 C6 C7 108.1(4) . . ?
C5 C6 C7 128.0(4) . . ?
C8 C7 C6 107.4(4) . . ?
C8 C7 H7 126.3 . . ?
C6 C7 H7 126.3 . . ?
C7 C8 C9 107.0(4) . . ?
C7 C8 H8 126.5 . . ?
C9 C8 H8 126.5 . . ?
N2 C9 C8 110.7(4) . . ?
N2 C9 C18 119.4(4) . . ?
C8 C9 C18 129.5(4) . . ?
C15 C10 C11 119.2(4) . . ?
C15 C10 C5 121.4(4) . . ?
C11 C10 C5 119.4(4) . . ?
C12 C11 C10 120.7(5) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 119.3(5) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C14 C13 C12 119.9(4) . . ?
C14 C13 C16 118.1(5) . . ?
C12 C13 C16 122.0(5) . . ?
C13 C14 C15 120.1(5) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C10 C15 C14 120.9(5) . . ?
C10 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
O1 C16 O2 123.3(6) . . ?
O1 C16 C13 123.7(6) . . ?
O2 C16 C13 113.0(6) . . ?
O2 C17 H17A 109.5 . . ?
O2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 110.9(4) . . ?
N3 C18 C9 119.7(4) . . ?
C19 C18 C9 129.4(4) . . ?
C20 C19 C18 106.1(4) . . ?
C20 C19 H19 126.9 . . ?
C18 C19 H19 126.9 . . ?
C19 C20 C21 107.7(4) . . ?
C19 C20 H20 126.1 . . ?
C21 C20 H20 126.1 . . ?
N3 C21 C22 124.6(4) . . ?
N3 C21 C20 108.2(4) . . ?
C22 C21 C20 127.1(4) . . ?
C23 C22 C21 127.1(4) . . ?
C23 C22 C27 116.0(4) . . ?
C21 C22 C27 116.9(4) . . ?
C22 C23 N4 124.3(4) . . ?
C22 C23 C24 127.7(4) . . ?
N4 C23 C24 108.0(4) . . ?
C25 C24 C23 107.3(4) . . ?
C25 C24 H24 126.3 . . ?
C23 C24 H24 126.3 . . ?
C24 C25 C26 106.6(5) . . ?
C24 C25 H25 126.7 . . ?
C26 C25 H25 126.7 . . ?
N4 C26 C25 111.1(5) . . ?
N4 C26 H26 124.5 . . ?
C25 C26 H26 124.5 . . ?
C28 C27 C33A 114.5(6) . . ?
C28 C27 C33B 115.0(6) . . ?
C33A C27 C33B 37.2(7) . . ?
C28 C27 C22 121.0(4) . . ?
C33A C27 C22 120.5(6) . . ?
C33B C27 C22 121.3(6) . . ?
C27 C28 C29 122.4(5) . . ?
C27 C28 H28 118.8 . . ?
C29 C28 H28 118.8 . . ?
C30 C29 C28 120.5(5) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C32A 116.1(7) . . ?
C29 C30 C32B 116.5(6) . . ?
C32A C30 C32B 35.3(7) . . ?
C29 C30 C33 119.1(4) . . ?
C32A C30 C33 121.6(6) . . ?
C32B C30 C33 121.3(6) . . ?
C30 C32A C33A 120.7(11) . . ?
C30 C32A H32A 119.7 . . ?
C33A C32A H32A 119.7 . . ?
C27 C33A C32A 120.1(11) . . ?
C27 C33A H33A 119.9 . . ?
C32A C33A H33A 119.9 . . ?
C33B C32B C30 118.1(10) . . ?
C33B C32B H32B 121.0 . . ?
C30 C32B H32B 121.0 . . ?
C32B C33B C27 120.6(10) . . ?
C32B C33B H33B 119.7 . . ?
C27 C33B H33B 119.7 . . ?
O3 C33 O4 122.8(4) . . ?
O3 C33 C30 124.8(5) . . ?
O4 C33 C30 112.3(4) . . ?
O4 C34 H34A 109.5 . . ?
O4 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O4 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C1 N1 C4 107.1(3) . . ?
C1 N1 Zn1 127.2(3) . . ?
C4 N1 Zn1 125.1(3) . . ?
C9 N2 C6 106.7(3) . . ?
C9 N2 Zn1 125.2(3) . . ?
C6 N2 Zn1 123.0(3) . . ?
C18 N3 C21 107.1(4) . . ?
C18 N3 Zn1 125.9(3) . 2_655 ?
C21 N3 Zn1 123.9(3) . 2_655 ?
C26 N4 C23 107.0(4) . . ?
C26 N4 Zn1 127.8(3) . 2_655 ?
C23 N4 Zn1 125.1(3) . 2_655 ?
C16 O2 C17 115.1(6) . . ?
C33 O4 C34 116.3(4) . . ?
N1 Zn1 N4 124.61(16) . 2_655 ?
N1 Zn1 N2 93.99(14) . . ?
N4 Zn1 N2 106.01(15) 2_655 . ?
N1 Zn1 N3 106.27(15) . 2_655 ?
N4 Zn1 N3 93.60(15) 2_655 2_655 ?
N2 Zn1 N3 136.53(15) . 2_655 ?
N5 C35 C36 111.2(5) . . ?
N5 C35 H35 124.4 . . ?
C36 C35 H35 124.4 . . ?
C37 C36 C35 107.0(5) . . ?
C37 C36 H36 126.5 . . ?
C35 C36 H36 126.5 . . ?
C36 C37 C38 107.7(4) . . ?
C36 C37 H37 126.2 . . ?
C38 C37 H37 126.2 . . ?
C39 C38 N5 124.6(4) . . ?
C39 C38 C37 127.4(4) . . ?
N5 C38 C37 107.9(4) . . ?
C38 C39 C40 126.2(4) . . ?
C38 C39 C44 116.2(4) . . ?
C40 C39 C44 117.5(4) . . ?
N6 C40 C39 125.6(4) . . ?
N6 C40 C41 108.3(4) . . ?
C39 C40 C41 126.0(4) . . ?
C42 C41 C40 107.4(4) . . ?
C42 C41 H41 126.3 . . ?
C40 C41 H41 126.3 . . ?
C41 C42 C43 106.5(4) . . ?
C41 C42 H42 126.8 . . ?
C43 C42 H42 126.8 . . ?
N6 C43 C42 111.0(4) . . ?
N6 C43 C52 120.5(4) . . ?
C42 C43 C52 128.1(5) . . ?
C45 C44 C49 119.3(5) . . ?
C45 C44 C39 120.8(5) . . ?
C49 C44 C39 119.9(5) . . ?
C44 C45 C46 120.0(5) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C47 C46 C45 119.7(5) . . ?
C47 C46 H46 120.2 . . ?
C45 C46 H46 120.2 . . ?
C46 C47 C48 120.4(5) . . ?
C46 C47 C50 117.4(5) . . ?
C48 C47 C50 122.0(5) . . ?
C49 C48 C47 119.5(5) . . ?
C49 C48 H48 120.3 . . ?
C47 C48 H48 120.3 . . ?
C48 C49 C44 120.9(5) . . ?
C48 C49 H49 119.6 . . ?
C44 C49 H49 119.6 . . ?
O5 C50 O6 124.0(5) . . ?
O5 C50 C47 123.2(6) . . ?
O6 C50 C47 112.8(6) . . ?
O6 C51 H51A 109.5 . . ?
O6 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
O6 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N7 C52 C53 110.8(4) . . ?
N7 C52 C43 118.7(4) . . ?
C53 C52 C43 130.5(5) . . ?
C54 C53 C52 106.0(5) . . ?
C54 C53 H53 127.0 . . ?
C52 C53 H53 127.0 . . ?
C53 C54 C55 108.2(4) . . ?
C53 C54 H54 125.9 . . ?
C55 C54 H54 125.9 . . ?
C56 C55 N7 124.4(4) . . ?
C56 C55 C54 127.3(4) . . ?
N7 C55 C54 108.3(4) . . ?
C55 C56 C57 127.3(4) . . ?
C55 C56 C61 116.3(5) . . ?
C57 C56 C61 116.4(5) . . ?
N8 C57 C56 124.0(5) . . ?
N8 C57 C58 107.5(5) . . ?
C56 C57 C58 128.4(5) . . ?
C59 C58 C57 107.3(5) . . ?
C59 C58 H58 126.4 . . ?
C57 C58 H58 126.4 . . ?
C58 C59 C60 106.2(5) . . ?
C58 C59 H59 126.9 . . ?
C60 C59 H59 126.9 . . ?
N8 C60 C59 111.6(5) . . ?
N8 C60 H60 124.2 . . ?
C59 C60 H60 124.2 . . ?
C66 C61 C62A 115.6(9) . . ?
C66 C61 C62B 117.1(10) . . ?
C62A C61 C62B 34(2) . . ?
C66 C61 C56 121.9(5) . . ?
C62A C61 C56 120.1(8) . . ?
C62B C61 C56 118.1(11) . . ?
C61 C62A C63A 124.6(16) . . ?
C61 C62A H62A 117.7 . . ?
C63A C62A H62A 117.7 . . ?
C64 C63A C62A 114.2(17) . . ?
C64 C63A H63A 122.9 . . ?
C62A C63A H63A 122.9 . . ?
C61 C62B C63B 114(2) . . ?
C61 C62B H62B 123.2 . . ?
C63B C62B H62B 123.2 . . ?
C64 C63B C62B 124.9(16) . . ?
C64 C63B H63B 117.5 . . ?
C62B C63B H63B 117.5 . . ?
C65 C64 C63B 113.9(11) . . ?
C65 C64 C63A 121.1(9) . . ?
C63B C64 C63A 31.1(12) . . ?
C65 C64 C67 119.2(5) . . ?
C63B C64 C67 123.6(8) . . ?
C63A C64 C67 118.2(9) . . ?
C64 C65 C66 120.6(5) . . ?
C64 C65 H65 119.7 . . ?
C66 C65 H65 119.7 . . ?
C61 C66 C65 121.1(5) . . ?
C61 C66 H66 119.5 . . ?
C65 C66 H66 119.5 . . ?
O7 C67 O8 123.3(5) . . ?
O7 C67 C64 123.6(6) . . ?
O8 C67 C64 113.1(5) . . ?
O8 C68 H68A 109.5 . . ?
O8 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
O8 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
N9 C69 C70 111.6(5) . . ?
N9 C69 H69 124.2 . . ?
C70 C69 H69 124.2 . . ?
C71 C70 C69 105.9(5) . . ?
C71 C70 H70 127.1 . . ?
C69 C70 H70 127.1 . . ?
C70 C71 C72 107.6(5) . . ?
C70 C71 H71 126.2 . . ?
C72 C71 H71 126.2 . . ?
N9 C72 C73 124.7(5) . . ?
N9 C72 C71 107.8(5) . . ?
C73 C72 C71 127.5(5) . . ?
C72 C73 C74 125.2(4) . . ?
C72 C73 C78 116.9(5) . . ?
C74 C73 C78 117.9(5) . . ?
N10 C74 C73 125.3(5) . . ?
N10 C74 C75 107.6(4) . . ?
C73 C74 C75 126.9(4) . . ?
C76 C75 C74 108.2(4) . . ?
C76 C75 H75 125.9 . . ?
C74 C75 H75 125.9 . . ?
C75 C76 C77 105.5(5) . . ?
C75 C76 H76 127.3 . . ?
C77 C76 H76 127.3 . . ?
N10 C77 C76 111.7(4) . . ?
N10 C77 C86 119.6(4) . . ?
C76 C77 C86 128.7(5) . . ?
C79 C78 C83 119.2(5) . . ?
C79 C78 C73 119.8(5) . . ?
C83 C78 C73 121.0(5) . . ?
C78 C79 C80 120.6(6) . . ?
C78 C79 H79 119.7 . . ?
C80 C79 H79 119.7 . . ?
C81 C80 C79 120.0(6) . . ?
C81 C80 H80 120.0 . . ?
C79 C80 H80 120.0 . . ?
C82 C81 C80 119.6(5) . . ?
C82 C81 C84 123.4(6) . . ?
C80 C81 C84 116.9(6) . . ?
C81 C82 C83 121.1(6) . . ?
C81 C82 H82 119.4 . . ?
C83 C82 H82 119.4 . . ?
C78 C83 C82 119.4(5) . . ?
C78 C83 H83 120.3 . . ?
C82 C83 H83 120.3 . . ?
O9 C84 O10 122.7(6) . . ?
O9 C84 C81 126.2(7) . . ?
O10 C84 C81 111.1(6) . . ?
O10 C85 H85A 109.5 . . ?
O10 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
O10 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
N11 C86 C87 111.9(4) . . ?
N11 C86 C77 119.2(4) . . ?
C87 C86 C77 128.7(5) . . ?
C88 C87 C86 106.7(5) . . ?
C88 C87 H87 126.7 . . ?
C86 C87 H87 126.7 . . ?
C87 C88 C89 106.6(4) . . ?
C87 C88 H88 126.7 . . ?
C89 C88 H88 126.7 . . ?
N11 C89 C90 124.1(4) . . ?
N11 C89 C88 108.8(4) . . ?
C90 C89 C88 127.1(4) . . ?
C91 C90 C89 127.1(4) . . ?
C91 C90 C95 117.5(4) . . ?
C89 C90 C95 115.3(4) . . ?
C90 C91 N12 123.5(4) . . ?
C90 C91 C92 127.6(5) . . ?
N12 C91 C92 108.9(4) . . ?
C93 C92 C91 106.8(5) . . ?
C93 C92 H92 126.6 . . ?
C91 C92 H92 126.6 . . ?
C92 C93 C94 107.0(5) . . ?
C92 C93 H93 126.5 . . ?
C94 C93 H93 126.5 . . ?
N12 C94 C93 111.1(5) . . ?
N12 C94 H94 124.4 . . ?
C93 C94 H94 124.4 . . ?
C96 C95 C100 118.5(5) . . ?
C96 C95 C90 119.6(5) . . ?
C100 C95 C90 121.9(5) . . ?
C97 C96 C95 121.1(5) . . ?
C97 C96 H96 119.4 . . ?
C95 C96 H96 119.4 . . ?
C96 C97 C98 120.4(5) . . ?
C96 C97 H97 119.8 . . ?
C98 C97 H97 119.8 . . ?
C99 C98 C97 119.3(5) . . ?
C99 C98 C101 122.4(6) . . ?
C97 C98 C101 118.2(6) . . ?
C98 C99 C100 120.8(5) . . ?
C98 C99 H99 119.6 . . ?
C100 C99 H99 119.6 . . ?
C99 C100 C95 119.8(5) . . ?
C99 C100 H100 120.1 . . ?
C95 C100 H100 120.1 . . ?
O11 C101 O12 122.3(6) . . ?
O11 C101 C98 123.5(6) . . ?
O12 C101 C98 114.2(6) . . ?
O12 C102 H10A 109.5 . . ?
O12 C102 H10B 109.5 . . ?
H10A C102 H10B 109.5 . . ?
O12 C102 H10C 109.5 . . ?
H10A C102 H10C 109.5 . . ?
H10B C102 H10C 109.5 . . ?
C35 N5 C38 106.2(4) . . ?
C35 N5 Zn2 129.0(3) . . ?
C38 N5 Zn2 124.8(3) . . ?
C43 N6 C40 106.7(4) . . ?
C43 N6 Zn2 126.4(3) . . ?
C40 N6 Zn2 123.2(3) . . ?
C52 N7 C55 106.8(4) . . ?
C52 N7 Zn3 126.3(3) . . ?
C55 N7 Zn3 125.2(3) . . ?
C60 N8 C57 107.3(4) . . ?
C60 N8 Zn3 127.2(4) . . ?
C57 N8 Zn3 125.5(4) . . ?
C69 N9 C72 107.0(4) . . ?
C69 N9 Zn2 126.2(4) . . ?
C72 N9 Zn2 126.5(3) . . ?
C77 N10 C74 106.9(4) . . ?
C77 N10 Zn2 125.6(3) . . ?
C74 N10 Zn2 125.6(3) . . ?
C86 N11 C89 105.8(4) . . ?
C86 N11 Zn3 125.4(3) . . ?
C89 N11 Zn3 122.3(3) . . ?
C94 N12 C91 106.2(4) . . ?
C94 N12 Zn3 127.7(3) . . ?
C91 N12 Zn3 125.2(3) . . ?
C50 O6 C51 113.3(5) . . ?
C67 O8 C68 117.6(5) . . ?
C84 O10 C85 116.6(6) . . ?
C101 O12 C102 110.5(7) . . ?
N5 Zn2 N9 122.45(17) . . ?
N5 Zn2 N10 111.40(16) . . ?
N9 Zn2 N10 92.18(17) . . ?
N5 Zn2 N6 93.58(16) . . ?
N9 Zn2 N6 103.04(17) . . ?
N10 Zn2 N6 137.42(17) . . ?
N12 Zn3 N7 109.85(16) . . ?
N12 Zn3 N11 93.27(16) . . ?
N7 Zn3 N11 135.75(17) . . ?
N12 Zn3 N8 130.76(19) . . ?
N7 Zn3 N8 92.49(17) . . ?
N11 Zn3 N8 100.28(18) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        29.42
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.143
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound5b
_database_code_depnum_ccdc_archive 'CCDC 1040044'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C102 H72 N12 O12 Zn3, 3(C H Cl3) '
_chemical_formula_sum            'C105 H75 Cl9 N12 O12 Zn3'
_chemical_formula_weight         2211.93

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                   18.1355(4)
_cell_length_b                   21.5289(5)
_cell_length_c                   25.5659(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.0080(10)
_cell_angle_gamma                90.00
_cell_volume                     9830.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9287
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      26.39

_exptl_crystal_description       prism
_exptl_crystal_colour            dark-purple
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4512
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9031
_exptl_absorpt_correction_T_max  0.9214
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
The EADP command was used for some atoms of one of the ester groups.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57850
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         30.12
_reflns_number_total             14449
_reflns_number_gt                8518
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0983P)²+11.9448P] 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         14449
_refine_ls_number_parameters     645
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0615
_refine_ls_wR_factor_ref         0.2011
_refine_ls_wR_factor_gt          0.1619
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.002
_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
C1 C 0.3682(2) 0.68660(19) 0.07207(15) 0.0414(9) Uani 1 1 d . . .
H1 H 0.3324 0.6642 0.0862 0.050 Uiso 1 1 calc R . .
C2 C 0.3985(3) 0.6679(2) 0.02734(16) 0.0483(11) Uani 1 1 d . . .
H2 H 0.3867 0.6322 0.0072 0.058 Uiso 1 1 calc R . .
C3 C 0.4484(2) 0.71245(18) 0.01963(15) 0.0415(9) Uani 1 1 d . . .
H3 H 0.4773 0.7131 -0.0071 0.050 Uiso 1 1 calc R . .
C4 C 0.44821(19) 0.75793(17) 0.05993(13) 0.0306(7) Uani 1 1 d . . .
C5 C 0.48751(19) 0.81371(17) 0.06597(13) 0.0292(7) Uani 1 1 d . . .
C6 C 0.47927(18) 0.86294(16) 0.10116(13) 0.0303(7) Uani 1 1 d . . .
C7 C 0.5200(2) 0.91902(18) 0.10541(15) 0.0393(9) Uani 1 1 d . . .
H7 H 0.5586 0.9289 0.0873 0.047 Uiso 1 1 calc R . .
C8 C 0.4927(2) 0.95631(18) 0.14095(15) 0.0392(9) Uani 1 1 d . . .
H8 H 0.5086 0.9962 0.1512 0.047 Uiso 1 1 calc R . .
C9 C 0.43550(18) 0.92194(16) 0.15889(13) 0.0289(7) Uani 1 1 d . . .
C10 C 0.54322(19) 0.82366(17) 0.02983(13) 0.0322(8) Uani 1 1 d . . .
C11 C 0.6091(2) 0.7919(2) 0.03773(17) 0.0517(12) Uani 1 1 d . . .
H11 H 0.6198 0.7644 0.0661 0.062 Uiso 1 1 calc R . .
C12 C 0.6605(3) 0.8000(2) 0.00400(17) 0.0547(12) Uani 1 1 d . . .
H12 H 0.7052 0.7778 0.0099 0.066 Uiso 1 1 calc R . .
C13 C 0.6463(2) 0.84061(18) -0.03806(14) 0.0339(8) Uani 1 1 d . . .
C14 C 0.5796(2) 0.8725(2) -0.04610(16) 0.0455(10) Uani 1 1 d . . .
H14 H 0.5688 0.8998 -0.0745 0.055 Uiso 1 1 calc R . .
C15 C 0.5282(2) 0.8643(2) -0.01231(16) 0.0483(11) Uani 1 1 d . . .
H15 H 0.4834 0.8863 -0.0182 0.058 Uiso 1 1 calc R . .
C16 C 0.7023(2) 0.84851(19) -0.07333(15) 0.0388(9) Uani 1 1 d . . .
C17 C 0.7317(3) 0.8995(2) -0.14783(19) 0.0596(13) Uani 1 1 d . . .
H17A H 0.7784 0.9140 -0.1281 0.089 Uiso 1 1 calc R . .
H17B H 0.7113 0.9304 -0.1733 0.089 Uiso 1 1 calc R . .
H17C H 0.7399 0.8618 -0.1660 0.089 Uiso 1 1 calc R . .
C18 C 0.38602(18) 0.94410(15) 0.19395(13) 0.0284(7) Uani 1 1 d . . .
C19 C 0.31225(19) 0.92306(16) 0.19500(14) 0.0321(7) Uani 1 1 d . . .
H19 H 0.2869 0.8916 0.1744 0.039 Uiso 1 1 calc R . .
C20 C 0.2855(2) 0.95816(16) 0.23233(15) 0.0337(8) Uani 1 1 d . . .
H20 H 0.2386 0.9546 0.2420 0.040 Uiso 1 1 calc R . .
C21 C 0.34260(18) 1.00099(15) 0.25366(13) 0.0285(7) Uani 1 1 d . . .
C22 C 0.33566(18) 1.04759(15) 0.29025(13) 0.0283(7) Uani 1 1 d . . .
C23 C 0.38786(19) 1.09278(16) 0.31022(14) 0.0314(7) Uani 1 1 d . . .
C24 C 0.3801(2) 1.14312(17) 0.34504(16) 0.0383(8) Uani 1 1 d . . .
H24 H 0.3379 1.1526 0.3596 0.046 Uiso 1 1 calc R . .
C25 C 0.4464(2) 1.17479(19) 0.35300(18) 0.0486(10) Uani 1 1 d . . .
H25 H 0.4580 1.2102 0.3737 0.058 Uiso 1 1 calc R . .
C26 C 0.4938(2) 1.14323(18) 0.32374(18) 0.0449(10) Uani 1 1 d . . .
H26 H 0.5428 1.1550 0.3225 0.054 Uiso 1 1 calc R . .
C27 C 0.26274(19) 1.04989(16) 0.31075(14) 0.0313(7) Uani 1 1 d . . .
C28 C 0.2535(2) 1.0120(2) 0.35276(17) 0.0484(10) Uani 1 1 d . . .
H28 H 0.2918 0.9854 0.3676 0.058 Uiso 1 1 calc R . .
C29 C 0.1875(3) 1.0135(2) 0.37301(19) 0.0530(11) Uani 1 1 d . . .
H29 H 0.1824 0.9888 0.4020 0.064 Uiso 1 1 calc R . .
C30 C 0.1299(2) 1.05093(19) 0.35065(19) 0.0493(11) Uani 1 1 d . . .
C31 C 0.1391(3) 1.0892(2) 0.3084(2) 0.0574(13) Uani 1 1 d . . .
H31 H 0.1004 1.1154 0.2933 0.069 Uiso 1 1 calc R . .
C32 C 0.2053(2) 1.0886(2) 0.28881(17) 0.0467(10) Uani 1 1 d . . .
H32 H 0.2112 1.1144 0.2607 0.056 Uiso 1 1 calc R . .
C33 C 0.0605(4) 1.0496(3) 0.3739(4) 0.1069(19) Uani 1 1 d . . .
C34 C -0.0640(4) 1.0781(3) 0.3659(3) 0.1069(19) Uani 1 1 d . . .
H34A H -0.0726 1.0375 0.3791 0.160 Uiso 1 1 calc R . .
H34B H -0.1060 1.0901 0.3396 0.160 Uiso 1 1 calc R . .
H34C H -0.0577 1.1074 0.3946 0.160 Uiso 1 1 calc R . .
C35 C 0.2138(2) 0.79648(18) 0.10706(14) 0.0361(8) Uani 1 1 d . . .
H35 H 0.2215 0.7963 0.0720 0.043 Uiso 1 1 calc R . .
C36 C 0.1459(2) 0.8132(2) 0.12279(16) 0.0427(9) Uani 1 1 d . . .
H36 H 0.1019 0.8252 0.1007 0.051 Uiso 1 1 calc R . .
C37 C 0.1574(2) 0.80825(18) 0.17665(15) 0.0377(8) Uani 1 1 d . . .
H37 H 0.1227 0.8172 0.1984 0.045 Uiso 1 1 calc R . .
C38 C 0.23150(19) 0.78712(16) 0.19349(13) 0.0297(7) Uani 1 1 d . . .
C39 C 0.26913(19) 0.77565(16) 0.24483(13) 0.0298(7) Uani 1 1 d . . .
C40 C 0.34493(19) 0.75788(16) 0.26047(13) 0.0299(7) Uani 1 1 d . . .
C41 C 0.3783(2) 0.73796(18) 0.31163(14) 0.0363(8) Uani 1 1 d . . .
H41 H 0.3541 0.7326 0.3405 0.044 Uiso 1 1 calc R . .
C42 C 0.4528(2) 0.72796(18) 0.31129(14) 0.0368(8) Uani 1 1 d . . .
H42 H 0.4884 0.7139 0.3395 0.044 Uiso 1 1 calc R . .
C43 C 0.46501(19) 0.74324(17) 0.25951(13) 0.0313(7) Uani 1 1 d . . .
C44 C 0.2272(2) 0.78741(16) 0.28969(14) 0.0317(7) Uani 1 1 d . . .
C45 C 0.2562(2) 0.83022(18) 0.32862(14) 0.0363(8) Uani 1 1 d . . .
H45 H 0.3016 0.8496 0.3269 0.044 Uiso 1 1 calc R . .
C46 C 0.2190(2) 0.84459(18) 0.36983(15) 0.0382(9) Uani 1 1 d . . .
H46 H 0.2391 0.8731 0.3958 0.046 Uiso 1 1 calc R . .
C47 C 0.1506(2) 0.81555(18) 0.37183(15) 0.0392(9) Uani 1 1 d . . .
C48 C 0.1220(2) 0.77346(19) 0.33364(17) 0.0449(10) Uani 1 1 d . . .
H48 H 0.0763 0.7545 0.3353 0.054 Uiso 1 1 calc R . .
C49 C 0.1596(2) 0.75842(18) 0.29246(16) 0.0384(9) Uani 1 1 d . . .
H49 H 0.1397 0.7293 0.2670 0.046 Uiso 1 1 calc R . .
C50 C 0.1062(3) 0.83184(19) 0.41415(16) 0.0453(10) Uani 1 1 d . . .
C51 C 0.0986(3) 0.8953(3) 0.4878(2) 0.0720(16) Uani 1 1 d . . .
H51A H 0.0506 0.9114 0.4719 0.108 Uiso 1 1 calc R . .
H51B H 0.1266 0.9271 0.5090 0.108 Uiso 1 1 calc R . .
H51C H 0.0919 0.8605 0.5100 0.108 Uiso 1 1 calc R . .
N1 N 0.39701(16) 0.73992(14) 0.09142(11) 0.0317(6) Uani 1 1 d . . .
N2 N 0.42707(15) 0.86551(13) 0.13506(10) 0.0276(6) Uani 1 1 d . . .
N3 N 0.40465(15) 0.99103(13) 0.22877(11) 0.0272(6) Uani 1 1 d . . .
N4 N 0.45982(16) 1.09454(13) 0.29809(13) 0.0342(7) Uani 1 1 d . . .
N5 N 0.26544(16) 0.78103(14) 0.14844(11) 0.0318(6) Uani 1 1 d . . .
N6 N 0.39964(16) 0.75988(13) 0.22833(11) 0.0290(6) Uani 1 1 d . . .
O1 O 0.76053(18) 0.8215(2) -0.06864(13) 0.0757(12) Uani 1 1 d . . .
O2 O 0.68034(15) 0.88812(14) -0.11227(11) 0.0485(7) Uani 1 1 d . . .
O3 O 0.0549(2) 1.0250(2) 0.4155(2) 0.1002(11) Uani 1 1 d . . .
O4 O 0.0032(2) 1.0771(2) 0.3422(2) 0.1002(11) Uani 1 1 d . . .
O5 O 0.04758(18) 0.80806(15) 0.41798(12) 0.0536(8) Uani 1 1 d . . .
O6 O 0.1391(2) 0.87563(15) 0.44645(13) 0.0622(9) Uani 1 1 d . . .
Zn1 Zn 0.37581(2) 0.787601(18) 0.153266(14) 0.02737(12) Uani 1 1 d . . .
Zn2 Zn 0.5000 1.03649(2) 0.2500 0.02783(14) Uani 1 2 d S . .
C52 C 0.3222(4) 0.9368(3) 0.0248(3) 0.0869(18) Uani 1 1 d . . .
H52 H 0.3563 0.9289 0.0583 0.104 Uiso 1 1 calc R . .
Cl1 Cl 0.36485(18) 0.99028(12) -0.00979(10) 0.1689(12) Uani 1 1 d . . .
Cl2 Cl 0.31048(8) 0.86707(8) -0.00968(7) 0.0810(4) Uani 1 1 d . . .
Cl3 Cl 0.23890(14) 0.96167(12) 0.04077(13) 0.1533(10) Uani 1 1 d . . .
C53 C -0.0050(14) 0.9468(5) 0.2621(7) 0.069(4) Uani 0.50 1 d P A -1
H53 H -0.0162 0.9913 0.2586 0.083 Uiso 0.50 1 calc PR A -1
Cl4 Cl -0.0132(2) 0.92408(18) 0.32566(14) 0.1054(12) Uani 0.50 1 d P A -1
Cl5 Cl 0.0867(3) 0.9354(3) 0.2523(3) 0.138(2) Uani 0.50 1 d P A -1
Cl6 Cl -0.0657(3) 0.9092(3) 0.2165(2) 0.146(2) Uani 0.50 1 d P A -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
C1 N1 1.321(5) . ?
C1 C2 1.411(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.355(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.422(5) . ?
C3 H3 0.9300 . ?
C4 N1 1.386(4) . ?
C4 C5 1.391(5) . ?
C5 C6 1.415(5) . ?
C5 C10 1.498(4) . ?
C6 N2 1.391(4) . ?
C6 C7 1.410(5) . ?
C7 C8 1.368(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.414(5) . ?
C8 H8 0.9300 . ?
C9 N2 1.356(4) . ?
C9 C18 1.455(5) . ?
C10 C11 1.362(5) . ?
C10 C15 1.377(5) . ?
C11 C12 1.387(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.375(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.374(5) . ?
C13 C16 1.480(5) . ?
C14 C15 1.389(5) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.193(5) . ?
C16 O2 1.319(5) . ?
C17 O2 1.432(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N3 1.350(4) . ?
C18 C19 1.417(5) . ?
C19 C20 1.370(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.422(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.392(5) . ?
C21 N3 1.402(4) . ?
C22 C23 1.391(5) . ?
C22 C27 1.505(4) . ?
C23 N4 1.393(4) . ?
C23 C24 1.425(5) . ?
C24 C25 1.366(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.408(6) . ?
C25 H25 0.9300 . ?
C26 N4 1.329(5) . ?
C26 H26 0.9300 . ?
C27 C32 1.375(5) . ?
C27 C28 1.381(5) . ?
C28 C29 1.385(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.364(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.392(6) . ?
C30 C33 1.481(6) . ?
C31 C32 1.380(5) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 O3 1.209(8) . ?
C33 O4 1.340(9) . ?
C34 O4 1.451(6) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 N5 1.328(5) . ?
C35 C36 1.406(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.361(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.414(5) . ?
C37 H37 0.9300 . ?
C38 C39 1.392(5) . ?
C38 N5 1.403(4) . ?
C39 C40 1.416(5) . ?
C39 C44 1.504(4) . ?
C40 N6 1.395(4) . ?
C40 C41 1.409(5) . ?
C41 C42 1.369(5) . ?
C41 H41 0.9300 . ?
C42 C43 1.418(5) . ?
C42 H42 0.9300 . ?
C43 N6 1.357(5) . ?
C43 C43 1.436(7) 2_655 ?
C44 C49 1.389(5) . ?
C44 C45 1.391(5) . ?
C45 C46 1.381(5) . ?
C45 H45 0.9300 . ?
C46 C47 1.398(5) . ?
C46 H46 0.9300 . ?
C47 C48 1.367(6) . ?
C47 C50 1.499(5) . ?
C48 C49 1.389(5) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
C50 O5 1.199(5) . ?
C50 O6 1.325(5) . ?
C51 O6 1.452(5) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
N1 Zn1 1.978(3) . ?
N2 Zn1 2.011(3) . ?
N3 Zn2 1.979(3) . ?
N4 Zn2 1.979(3) . ?
N5 Zn1 1.989(3) . ?
N6 Zn1 1.984(3) . ?
Zn2 N4 1.979(3) 2_655 ?
Zn2 N3 1.979(3) 2_655 ?
C52 Cl1 1.715(7) . ?
C52 Cl3 1.718(7) . ?
C52 Cl2 1.736(7) . ?
C52 H52 0.9800 . ?
C53 Cl6 1.67(2) . ?
C53 Cl4 1.729(15) . ?
C53 Cl5 1.74(2) . ?
C53 H53 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
N1 C1 C2 111.5(3) . . ?
N1 C1 H1 124.2 . . ?
C2 C1 H1 124.2 . . ?
C3 C2 C1 106.3(3) . . ?
C3 C2 H2 126.9 . . ?
C1 C2 H2 126.9 . . ?
C2 C3 C4 107.3(3) . . ?
C2 C3 H3 126.4 . . ?
C4 C3 H3 126.4 . . ?
N1 C4 C5 124.0(3) . . ?
N1 C4 C3 108.3(3) . . ?
C5 C4 C3 127.6(3) . . ?
C4 C5 C6 127.5(3) . . ?
C4 C5 C10 116.3(3) . . ?
C6 C5 C10 116.2(3) . . ?
N2 C6 C7 108.8(3) . . ?
N2 C6 C5 125.8(3) . . ?
C7 C6 C5 125.4(3) . . ?
C8 C7 C6 108.0(3) . . ?
C8 C7 H7 126.0 . . ?
C6 C7 H7 126.0 . . ?
C7 C8 C9 106.2(3) . . ?
C7 C8 H8 126.9 . . ?
C9 C8 H8 126.9 . . ?
N2 C9 C8 110.8(3) . . ?
N2 C9 C18 122.5(3) . . ?
C8 C9 C18 126.5(3) . . ?
C11 C10 C15 119.0(3) . . ?
C11 C10 C5 120.4(3) . . ?
C15 C10 C5 120.7(3) . . ?
C10 C11 C12 120.8(4) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C13 C12 C11 120.8(4) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C14 C13 C12 118.4(3) . . ?
C14 C13 C16 122.0(3) . . ?
C12 C13 C16 119.6(3) . . ?
C13 C14 C15 120.8(4) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C10 C15 C14 120.3(4) . . ?
C10 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
O1 C16 O2 122.5(3) . . ?
O1 C16 C13 124.9(4) . . ?
O2 C16 C13 112.6(3) . . ?
O2 C17 H17A 109.5 . . ?
O2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 110.8(3) . . ?
N3 C18 C9 122.8(3) . . ?
C19 C18 C9 126.3(3) . . ?
C20 C19 C18 106.6(3) . . ?
C20 C19 H19 126.7 . . ?
C18 C19 H19 126.7 . . ?
C19 C20 C21 107.6(3) . . ?
C19 C20 H20 126.2 . . ?
C21 C20 H20 126.2 . . ?
C22 C21 N3 126.0(3) . . ?
C22 C21 C20 125.5(3) . . ?
N3 C21 C20 108.3(3) . . ?
C23 C22 C21 128.0(3) . . ?
C23 C22 C27 115.6(3) . . ?
C21 C22 C27 116.4(3) . . ?
C22 C23 N4 122.8(3) . . ?
C22 C23 C24 128.8(3) . . ?
N4 C23 C24 108.4(3) . . ?
C25 C24 C23 107.0(3) . . ?
C25 C24 H24 126.5 . . ?
C23 C24 H24 126.5 . . ?
C24 C25 C26 106.4(3) . . ?
C24 C25 H25 126.8 . . ?
C26 C25 H25 126.8 . . ?
N4 C26 C25 111.7(3) . . ?
N4 C26 H26 124.1 . . ?
C25 C26 H26 124.1 . . ?
C32 C27 C28 119.3(3) . . ?
C32 C27 C22 121.8(3) . . ?
C28 C27 C22 119.0(3) . . ?
C27 C28 C29 120.5(4) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C30 C29 C28 120.4(4) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C31 119.2(4) . . ?
C29 C30 C33 117.5(5) . . ?
C31 C30 C33 123.2(5) . . ?
C32 C31 C30 120.4(4) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C27 C32 C31 120.2(4) . . ?
C27 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
O3 C33 O4 123.4(5) . . ?
O3 C33 C30 124.7(6) . . ?
O4 C33 C30 111.9(6) . . ?
O4 C34 H34A 109.5 . . ?
O4 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O4 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N5 C35 C36 111.6(3) . . ?
N5 C35 H35 124.2 . . ?
C36 C35 H35 124.2 . . ?
C37 C36 C35 106.4(4) . . ?
C37 C36 H36 126.8 . . ?
C35 C36 H36 126.8 . . ?
C36 C37 C38 107.6(3) . . ?
C36 C37 H37 126.2 . . ?
C38 C37 H37 126.2 . . ?
C39 C38 N5 123.0(3) . . ?
C39 C38 C37 129.0(3) . . ?
N5 C38 C37 108.0(3) . . ?
C38 C39 C40 127.4(3) . . ?
C38 C39 C44 117.3(3) . . ?
C40 C39 C44 115.1(3) . . ?
N6 C40 C41 108.7(3) . . ?
N6 C40 C39 125.5(3) . . ?
C41 C40 C39 125.7(3) . . ?
C42 C41 C40 107.9(3) . . ?
C42 C41 H41 126.0 . . ?
C40 C41 H41 126.0 . . ?
C41 C42 C43 106.5(3) . . ?
C41 C42 H42 126.8 . . ?
C43 C42 H42 126.8 . . ?
N6 C43 C42 110.3(3) . . ?
N6 C43 C43 122.3(4) . 2_655 ?
C42 C43 C43 127.3(4) . 2_655 ?
C49 C44 C45 119.2(3) . . ?
C49 C44 C39 122.1(3) . . ?
C45 C44 C39 118.6(3) . . ?
C46 C45 C44 121.4(3) . . ?
C46 C45 H45 119.3 . . ?
C44 C45 H45 119.3 . . ?
C45 C46 C47 118.8(3) . . ?
C45 C46 H46 120.6 . . ?
C47 C46 H46 120.6 . . ?
C48 C47 C46 120.0(3) . . ?
C48 C47 C50 119.0(4) . . ?
C46 C47 C50 120.9(4) . . ?
C47 C48 C49 121.3(3) . . ?
C47 C48 H48 119.3 . . ?
C49 C48 H48 119.3 . . ?
C48 C49 C44 119.2(4) . . ?
C48 C49 H49 120.4 . . ?
C44 C49 H49 120.4 . . ?
O5 C50 O6 124.2(3) . . ?
O5 C50 C47 123.7(4) . . ?
O6 C50 C47 112.1(3) . . ?
O6 C51 H51A 109.5 . . ?
O6 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
O6 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C1 N1 C4 106.6(3) . . ?
C1 N1 Zn1 129.1(2) . . ?
C4 N1 Zn1 124.2(2) . . ?
C9 N2 C6 106.2(3) . . ?
C9 N2 Zn1 131.6(2) . . ?
C6 N2 Zn1 120.2(2) . . ?
C18 N3 C21 106.6(3) . . ?
C18 N3 Zn2 131.1(2) . . ?
C21 N3 Zn2 122.1(2) . . ?
C26 N4 C23 106.4(3) . . ?
C26 N4 Zn2 128.0(3) . . ?
C23 N4 Zn2 125.5(2) . . ?
C35 N5 C38 106.3(3) . . ?
C35 N5 Zn1 126.5(2) . . ?
C38 N5 Zn1 121.5(2) . . ?
C43 N6 C40 106.5(3) . . ?
C43 N6 Zn1 132.0(2) . . ?
C40 N6 Zn1 121.4(2) . . ?
C16 O2 C17 116.5(3) . . ?
C33 O4 C34 112.0(5) . . ?
C50 O6 C51 115.6(3) . . ?
N1 Zn1 N6 125.25(12) . . ?
N1 Zn1 N5 104.29(12) . . ?
N6 Zn1 N5 94.95(12) . . ?
N1 Zn1 N2 94.93(11) . . ?
N6 Zn1 N2 116.29(11) . . ?
N5 Zn1 N2 123.06(12) . . ?
N4 Zn2 N4 101.67(18) 2_655 . ?
N4 Zn2 N3 94.83(11) 2_655 2_655 ?
N4 Zn2 N3 122.72(12) . 2_655 ?
N4 Zn2 N3 122.72(12) 2_655 . ?
N4 Zn2 N3 94.83(11) . . ?
N3 Zn2 N3 120.73(16) 2_655 . ?
Cl1 C52 Cl3 114.1(4) . . ?
Cl1 C52 Cl2 110.1(4) . . ?
Cl3 C52 Cl2 110.8(4) . . ?
Cl1 C52 H52 107.2 . . ?
Cl3 C52 H52 107.2 . . ?
Cl2 C52 H52 107.2 . . ?
Cl6 C53 Cl4 111.5(8) . . ?
Cl6 C53 Cl5 111.2(7) . . ?
Cl4 C53 Cl5 109.6(14) . . ?
Cl6 C53 H53 108.1 . . ?
Cl4 C53 H53 108.1 . . ?
Cl5 C53 H53 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.12
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.146
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.117
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compoundP-6b
_database_code_depnum_ccdc_archive 'CCDC 1040045'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C136 H96 N16 O16 Zn4'
_chemical_formula_weight         2471.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   I222

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

_cell_length_a                   15.3648(9)
_cell_length_b                   19.7305(11)
_cell_length_c                   23.6393(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7166.4(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    6036
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      27.78

_exptl_crystal_description       rod
_exptl_crystal_colour            dark-blue
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2544
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9056
_exptl_absorpt_correction_T_max  0.9717
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      190(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24227
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.34
_diffrn_reflns_theta_max         30.06
_reflns_number_total             10413
_reflns_number_gt                8208
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0407P)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   0.050(8)
_refine_ls_number_reflns         10413
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.0941
_refine_ls_wR_factor_gt          0.0899
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      0.953
_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
C1 C 0.66774(17) 0.20743(13) 0.40611(10) 0.0325(5) Uani 1 1 d . . .
H1 H 0.6354 0.2268 0.4352 0.039 Uiso 1 1 calc R . .
C2 C 0.64027(19) 0.20450(16) 0.34994(11) 0.0418(6) Uani 1 1 d . . .
H2 H 0.5885 0.2214 0.3352 0.050 Uiso 1 1 calc R . .
C3 C 0.70549(19) 0.17135(13) 0.32064(10) 0.0357(5) Uani 1 1 d . . .
H3 H 0.7058 0.1610 0.2823 0.043 Uiso 1 1 calc R . .
C4 C 0.77199(15) 0.15624(13) 0.36046(8) 0.0264(5) Uani 1 1 d . . .
C5 C 0.85092(15) 0.12352(12) 0.35076(9) 0.0251(5) Uani 1 1 d . . .
C6 C 0.91682(15) 0.10917(12) 0.39024(9) 0.0250(5) Uani 1 1 d . . .
C7 C 1.00276(16) 0.08753(13) 0.37707(10) 0.0326(5) Uani 1 1 d . . .
H7 H 1.0241 0.0777 0.3412 0.039 Uiso 1 1 calc R . .
C8 C 1.04809(16) 0.08384(13) 0.42633(10) 0.0316(5) Uani 1 1 d . . .
H8 H 1.1063 0.0718 0.4303 0.038 Uiso 1 1 calc R . .
C9 C 0.99039(14) 0.10175(11) 0.47023(9) 0.0249(5) Uani 1 1 d . . .
C10 C 0.86783(15) 0.09851(12) 0.29163(9) 0.0259(5) Uani 1 1 d . . .
C11 C 0.86282(18) 0.02938(13) 0.28158(10) 0.0350(6) Uani 1 1 d . . .
H11 H 0.8538 -0.0001 0.3117 0.042 Uiso 1 1 calc R . .
C12 C 0.8710(2) 0.00357(15) 0.22729(11) 0.0403(6) Uani 1 1 d . . .
H12 H 0.8666 -0.0428 0.2208 0.048 Uiso 1 1 calc R . .
C13 C 0.88600(17) 0.04806(13) 0.18282(10) 0.0328(5) Uani 1 1 d . . .
C14 C 0.8946(2) 0.11590(14) 0.19286(10) 0.0431(7) Uani 1 1 d . . .
H14 H 0.9072 0.1452 0.1631 0.052 Uiso 1 1 calc R . .
C15 C 0.8847(2) 0.14118(14) 0.24700(10) 0.0403(6) Uani 1 1 d . . .
H15 H 0.8894 0.1876 0.2533 0.048 Uiso 1 1 calc R . .
C16 C 0.8902(2) 0.02212(16) 0.12299(11) 0.0444(7) Uani 1 1 d . . .
C17 C 0.8735(3) -0.0733(2) 0.06413(14) 0.0882(14) Uani 1 1 d . . .
H17A H 0.8239 -0.0563 0.0439 0.132 Uiso 1 1 calc R . .
H17B H 0.8696 -0.1217 0.0669 0.132 Uiso 1 1 calc R . .
H17C H 0.9258 -0.0611 0.0444 0.132 Uiso 1 1 calc R . .
C18 C 0.8002(2) 0.29135(12) 0.53030(10) 0.0358(5) Uani 1 1 d . . .
H18 H 0.8149 0.3100 0.4955 0.043 Uiso 1 1 calc R . .
C19 C 0.7838(2) 0.32975(13) 0.57914(11) 0.0456(8) Uani 1 1 d . . .
H19 H 0.7855 0.3767 0.5825 0.055 Uiso 1 1 calc R . .
C20 C 0.76465(19) 0.28399(13) 0.62087(11) 0.0375(6) Uani 1 1 d . . .
H20 H 0.7517 0.2940 0.6584 0.045 Uiso 1 1 calc R . .
C21 C 0.76832(16) 0.21794(12) 0.59612(9) 0.0273(5) Uani 1 1 d . . .
C22 C 0.73947(15) 0.15808(12) 0.62002(9) 0.0252(5) Uani 1 1 d . . .
C23 C 0.72791(15) 0.09534(11) 0.59303(9) 0.0237(4) Uani 1 1 d . . .
C24 C 0.69931(18) 0.03422(11) 0.61935(9) 0.0275(4) Uani 1 1 d . . .
H24 H 0.6842 0.0290 0.6572 0.033 Uiso 1 1 calc R . .
C25 C 0.69808(18) -0.01493(11) 0.57921(9) 0.0289(5) Uani 1 1 d . . .
H25 H 0.6837 -0.0603 0.5847 0.035 Uiso 1 1 calc R . .
C26 C 0.72256(14) 0.01545(10) 0.52796(9) 0.0227(4) Uani 1 1 d . . .
C27 C 0.71182(15) 0.16055(11) 0.68071(8) 0.0252(5) Uani 1 1 d . . .
C28 C 0.62377(17) 0.16291(13) 0.69361(9) 0.0353(6) Uani 1 1 d . . .
H28 H 0.5830 0.1615 0.6645 0.042 Uiso 1 1 calc R . .
C29 C 0.59570(19) 0.16735(13) 0.74899(10) 0.0381(6) Uani 1 1 d . . .
H29 H 0.5365 0.1697 0.7570 0.046 Uiso 1 1 calc R . .
C30 C 0.65572(18) 0.16824(12) 0.79239(10) 0.0321(6) Uani 1 1 d . . .
C31 C 0.74270(19) 0.16369(13) 0.78029(10) 0.0377(6) Uani 1 1 d . . .
H31 H 0.7830 0.1628 0.8096 0.045 Uiso 1 1 calc R . .
C32 C 0.77131(17) 0.16033(14) 0.72428(10) 0.0359(6) Uani 1 1 d . . .
H32 H 0.8305 0.1580 0.7164 0.043 Uiso 1 1 calc R . .
C33 C 0.6282(2) 0.17513(14) 0.85294(11) 0.0407(6) Uani 1 1 d . . .
C34 C 0.5158(3) 0.2152(2) 0.91311(13) 0.0729(11) Uani 1 1 d . . .
H34A H 0.4539 0.2216 0.9118 0.109 Uiso 1 1 calc R . .
H34B H 0.5428 0.2550 0.9284 0.109 Uiso 1 1 calc R . .
H34C H 0.5291 0.1769 0.9367 0.109 Uiso 1 1 calc R . .
N1 N 0.74564(14) 0.17930(10) 0.41333(8) 0.0275(4) Uani 1 1 d . . .
N2 N 0.91074(12) 0.11778(10) 0.44890(7) 0.0239(4) Uani 1 1 d . . .
N3 N 0.79243(14) 0.22519(9) 0.53960(7) 0.0279(4) Uani 1 1 d . . .
N4 N 0.74075(12) 0.08214(9) 0.53540(7) 0.0205(4) Uani 1 1 d . . .
O1 O 0.9014(2) 0.05752(13) 0.08297(8) 0.0721(8) Uani 1 1 d . . .
O2 O 0.87503(18) -0.04434(12) 0.12006(9) 0.0617(6) Uani 1 1 d . . .
O3 O 0.67178(15) 0.16131(12) 0.89244(8) 0.0568(6) Uani 1 1 d . . .
O4 O 0.54843(15) 0.20301(12) 0.85613(8) 0.0561(6) Uani 1 1 d . . .
Zn1 Zn 0.800886(17) 0.149471(13) 0.485046(9) 0.02359(6) Uani 1 1 d . . .


_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
C1 N1 1.330(3) . ?
C1 C2 1.395(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.383(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.421(3) . ?
C3 H3 0.9300 . ?
C4 N1 1.390(3) . ?
C4 C5 1.393(3) . ?
C5 C6 1.406(3) . ?
C5 C10 1.505(3) . ?
C6 N2 1.400(3) . ?
C6 C7 1.422(3) . ?
C7 C8 1.359(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.410(3) . ?
C8 H8 0.9300 . ?
C9 N2 1.361(3) . ?
C9 C9 1.438(4) 3_756 ?
C10 C15 1.374(3) . ?
C10 C11 1.387(3) . ?
C11 C12 1.387(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.389(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.366(4) . ?
C13 C16 1.505(3) . ?
C14 C15 1.382(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.188(4) . ?
C16 O2 1.334(4) . ?
C17 O2 1.440(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N3 1.329(3) . ?
C18 C19 1.404(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.369(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.430(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.382(3) . ?
C21 N3 1.394(3) . ?
C22 C23 1.404(3) . ?
C22 C27 1.497(3) . ?
C23 N4 1.401(3) . ?
C23 C24 1.426(3) . ?
C24 C25 1.357(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.403(3) . ?
C25 H25 0.9300 . ?
C26 N4 1.357(3) . ?
C26 C26 1.456(4) 4_556 ?
C27 C32 1.377(3) . ?
C27 C28 1.388(3) . ?
C28 C29 1.381(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.380(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.370(4) . ?
C30 C33 1.499(3) . ?
C31 C32 1.397(3) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 O3 1.181(3) . ?
C33 O4 1.345(4) . ?
C34 O4 1.457(3) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
N1 Zn1 1.9852(19) . ?
N2 Zn1 1.9924(19) . ?
N3 Zn1 1.9780(18) . ?
N4 Zn1 2.0089(17) . ?

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 C1 C2 112.2(2) . . ?
N1 C1 H1 123.9 . . ?
C2 C1 H1 123.9 . . ?
C3 C2 C1 106.1(2) . . ?
C3 C2 H2 127.0 . . ?
C1 C2 H2 127.0 . . ?
C2 C3 C4 106.8(2) . . ?
C2 C3 H3 126.6 . . ?
C4 C3 H3 126.6 . . ?
N1 C4 C5 123.59(19) . . ?
N1 C4 C3 108.5(2) . . ?
C5 C4 C3 127.9(2) . . ?
C4 C5 C6 127.7(2) . . ?
C4 C5 C10 117.08(19) . . ?
C6 C5 C10 115.2(2) . . ?
N2 C6 C5 125.8(2) . . ?
N2 C6 C7 108.37(19) . . ?
C5 C6 C7 125.7(2) . . ?
C8 C7 C6 107.7(2) . . ?
C8 C7 H7 126.1 . . ?
C6 C7 H7 126.1 . . ?
C7 C8 C9 107.2(2) . . ?
C7 C8 H8 126.4 . . ?
C9 C8 H8 126.4 . . ?
N2 C9 C8 110.55(19) . . ?
N2 C9 C9 123.2(2) . 3_756 ?
C8 C9 C9 126.2(3) . 3_756 ?
C15 C10 C11 118.8(2) . . ?
C15 C10 C5 123.0(2) . . ?
C11 C10 C5 118.2(2) . . ?
C12 C11 C10 121.0(2) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 118.9(3) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C14 C13 C12 120.3(2) . . ?
C14 C13 C16 119.5(2) . . ?
C12 C13 C16 120.2(2) . . ?
C13 C14 C15 120.3(2) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C10 C15 C14 120.7(2) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
O1 C16 O2 124.2(3) . . ?
O1 C16 C13 123.7(3) . . ?
O2 C16 C13 112.1(2) . . ?
O2 C17 H17A 109.5 . . ?
O2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 112.2(2) . . ?
N3 C18 H18 123.9 . . ?
C19 C18 H18 123.9 . . ?
C20 C19 C18 106.0(2) . . ?
C20 C19 H19 127.0 . . ?
C18 C19 H19 127.0 . . ?
C19 C20 C21 107.3(2) . . ?
C19 C20 H20 126.3 . . ?
C21 C20 H20 126.3 . . ?
C22 C21 N3 124.4(2) . . ?
C22 C21 C20 126.8(2) . . ?
N3 C21 C20 108.0(2) . . ?
C21 C22 C23 127.46(19) . . ?
C21 C22 C27 117.1(2) . . ?
C23 C22 C27 115.4(2) . . ?
N4 C23 C22 126.0(2) . . ?
N4 C23 C24 108.09(18) . . ?
C22 C23 C24 125.89(19) . . ?
C25 C24 C23 107.67(19) . . ?
C25 C24 H24 126.2 . . ?
C23 C24 H24 126.2 . . ?
C24 C25 C26 107.14(19) . . ?
C24 C25 H25 126.4 . . ?
C26 C25 H25 126.4 . . ?
N4 C26 C25 110.95(18) . . ?
N4 C26 C26 121.6(2) . 4_556 ?
C25 C26 C26 127.2(2) . 4_556 ?
C32 C27 C28 118.9(2) . . ?
C32 C27 C22 121.9(2) . . ?
C28 C27 C22 119.2(2) . . ?
C29 C28 C27 121.0(2) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C30 C29 C28 119.8(3) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C31 C30 C29 119.7(2) . . ?
C31 C30 C33 118.7(2) . . ?
C29 C30 C33 121.5(3) . . ?
C30 C31 C32 120.5(2) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C27 C32 C31 120.0(2) . . ?
C27 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
O3 C33 O4 124.5(3) . . ?
O3 C33 C30 125.0(3) . . ?
O4 C33 C30 110.4(2) . . ?
O4 C34 H34A 109.5 . . ?
O4 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O4 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C1 N1 C4 106.45(19) . . ?
C1 N1 Zn1 128.16(17) . . ?
C4 N1 Zn1 123.10(16) . . ?
C9 N2 C6 106.18(17) . . ?
C9 N2 Zn1 132.52(14) . . ?
C6 N2 Zn1 121.29(14) . . ?
C18 N3 C21 106.46(19) . . ?
C18 N3 Zn1 128.90(15) . . ?
C21 N3 Zn1 124.40(15) . . ?
C26 N4 C23 106.11(17) . . ?
C26 N4 Zn1 131.25(14) . . ?
C23 N4 Zn1 121.20(14) . . ?
C16 O2 C17 116.1(3) . . ?
C33 O4 C34 115.7(3) . . ?
N3 Zn1 N1 107.75(8) . . ?
N3 Zn1 N2 124.91(8) . . ?
N1 Zn1 N2 95.11(8) . . ?
N3 Zn1 N4 94.76(7) . . ?
N1 Zn1 N4 120.36(8) . . ?
N2 Zn1 N4 115.86(8) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.06
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.062

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 0.500 0.006 906 356 ' '
2 0.099 0.265 0.281 7 1 ' '
3 0.099 0.735 0.719 8 0 ' '
4 0.500 0.000 0.190 906 356 ' '
5 0.400 0.235 0.781 8 0 ' '
6 0.400 0.765 0.219 7 1 ' '
7 0.599 0.235 0.219 8 0 ' '
8 0.599 0.765 0.781 7 1 ' '
9 0.900 0.265 0.719 7 1 ' '
10 0.900 0.735 0.281 8 0 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compoundM-6b
_database_code_depnum_ccdc_archive 'CCDC 1040046'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C136 H96 N16 O16 Zn4'
_chemical_formula_weight         2471.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   I222

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

_cell_length_a                   15.3370(6)
_cell_length_b                   19.7279(14)
_cell_length_c                   23.6518(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7156.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    9679
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      26.79

_exptl_crystal_description       rod
_exptl_crystal_colour            dark-blue
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2544
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9311
_exptl_absorpt_correction_T_max  0.9786
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      190(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50642
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.34
_diffrn_reflns_theta_max         30.07
_reflns_number_total             10481
_reflns_number_gt                7662
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0520P)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   0.067(9)
_refine_ls_number_reflns         10481
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.1021
_refine_ls_wR_factor_gt          0.0958
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      0.954
_refine_ls_shift/su_max          0.002
_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
C1 C 0.6999(2) 0.70882(13) 0.46975(10) 0.0366(6) Uani 1 1 d . . .
H1 H 0.6859 0.6901 0.5047 0.044 Uiso 1 1 calc R . .
C2 C 0.7159(2) 0.67035(15) 0.42081(12) 0.0458(8) Uani 1 1 d . . .
H2 H 0.7139 0.6234 0.4174 0.055 Uiso 1 1 calc R . .
C3 C 0.73515(19) 0.71640(14) 0.37918(11) 0.0375(6) Uani 1 1 d . . .
H3 H 0.7480 0.7065 0.3417 0.045 Uiso 1 1 calc R . .
C4 C 0.73179(17) 0.78220(13) 0.40387(9) 0.0277(5) Uani 1 1 d . . .
C5 C 0.76065(15) 0.84216(14) 0.38016(9) 0.0259(5) Uani 1 1 d . . .
C6 C 0.77211(15) 0.90444(13) 0.40690(9) 0.0242(5) Uani 1 1 d . . .
C7 C 0.80089(18) 0.96560(12) 0.38060(9) 0.0288(5) Uani 1 1 d . . .
H7 H 0.8160 0.9708 0.3428 0.035 Uiso 1 1 calc R . .
C8 C 0.80234(19) 1.01496(12) 0.42068(9) 0.0298(5) Uani 1 1 d . . .
H8 H 0.8169 1.0603 0.4153 0.036 Uiso 1 1 calc R . .
C9 C 0.77742(15) 0.98391(12) 0.47221(9) 0.0248(5) Uani 1 1 d . . .
C10 C 0.78858(17) 0.83915(12) 0.31938(9) 0.0273(5) Uani 1 1 d . . .
C11 C 0.72903(18) 0.83923(15) 0.27599(10) 0.0372(7) Uani 1 1 d . . .
H11 H 0.6697 0.8413 0.2840 0.045 Uiso 1 1 calc R . .
C12 C 0.7575(2) 0.83623(15) 0.21962(10) 0.0402(7) Uani 1 1 d . . .
H12 H 0.7171 0.8374 0.1903 0.048 Uiso 1 1 calc R . .
C13 C 0.84445(19) 0.83158(14) 0.20776(10) 0.0336(6) Uani 1 1 d . . .
C14 C 0.90426(19) 0.83265(15) 0.25115(10) 0.0389(7) Uani 1 1 d . . .
H14 H 0.9636 0.8303 0.2432 0.047 Uiso 1 1 calc R . .
C15 C 0.87625(19) 0.83721(15) 0.30660(10) 0.0381(7) Uani 1 1 d . . .
H15 H 0.9171 0.8390 0.3356 0.046 Uiso 1 1 calc R . .
C16 C 0.8718(2) 0.82492(15) 0.14722(11) 0.0403(7) Uani 1 1 d . . .
C17 C 0.9835(3) 0.7845(2) 0.08701(14) 0.0743(12) Uani 1 1 d . . .
H17A H 0.9487 0.7500 0.0694 0.111 Uiso 1 1 calc R . .
H17B H 1.0431 0.7699 0.0886 0.111 Uiso 1 1 calc R . .
H17C H 0.9796 0.8256 0.0654 0.111 Uiso 1 1 calc R . .
C18 C 0.83193(18) 0.79236(15) 0.59366(11) 0.0346(6) Uani 1 1 d . . .
H18 H 0.8642 0.7728 0.5647 0.042 Uiso 1 1 calc R . .
C19 C 0.85934(19) 0.79555(17) 0.65019(11) 0.0416(7) Uani 1 1 d . . .
H19 H 0.9113 0.7788 0.6649 0.050 Uiso 1 1 calc R . .
C20 C 0.79452(19) 0.82826(14) 0.67953(10) 0.0360(6) Uani 1 1 d . . .
H20 H 0.7942 0.8385 0.7179 0.043 Uiso 1 1 calc R . .
C21 C 0.72802(15) 0.84342(14) 0.63965(9) 0.0265(5) Uani 1 1 d . . .
C22 C 0.64929(15) 0.87633(13) 0.64943(9) 0.0267(5) Uani 1 1 d . . .
C23 C 0.58273(16) 0.89102(13) 0.60966(9) 0.0271(5) Uani 1 1 d . . .
C24 C 0.49760(17) 0.91245(15) 0.62331(10) 0.0325(6) Uani 1 1 d . . .
H24 H 0.4765 0.9222 0.6593 0.039 Uiso 1 1 calc R . .
C25 C 0.45193(17) 0.91626(15) 0.57377(10) 0.0335(6) Uani 1 1 d . . .
H25 H 0.3937 0.9285 0.5698 0.040 Uiso 1 1 calc R . .
C26 C 0.50914(15) 0.89825(13) 0.53004(9) 0.0274(5) Uani 1 1 d . . .
C27 C 0.63167(16) 0.90172(13) 0.70835(9) 0.0278(5) Uani 1 1 d . . .
C28 C 0.63711(18) 0.97074(14) 0.71813(10) 0.0360(6) Uani 1 1 d . . .
H28 H 0.6462 1.0002 0.6880 0.043 Uiso 1 1 calc R . .
C29 C 0.6290(2) 0.99641(16) 0.77259(12) 0.0424(7) Uani 1 1 d . . .
H29 H 0.6335 1.0428 0.7791 0.051 Uiso 1 1 calc R . .
C30 C 0.61423(17) 0.95208(15) 0.81730(10) 0.0350(6) Uani 1 1 d . . .
C31 C 0.6058(2) 0.88443(16) 0.80700(10) 0.0452(7) Uani 1 1 d . . .
H31 H 0.5936 0.8551 0.8367 0.054 Uiso 1 1 calc R . .
C32 C 0.6152(2) 0.85889(16) 0.75300(10) 0.0418(7) Uani 1 1 d . . .
H32 H 0.6103 0.8125 0.7468 0.050 Uiso 1 1 calc R . .
C33 C 0.6100(2) 0.97803(18) 0.87675(11) 0.0465(8) Uani 1 1 d . . .
C34 C 0.6261(3) 1.0727(2) 0.93614(15) 0.0892(15) Uani 1 1 d . . .
H34A H 0.5726 1.0617 0.9552 0.134 Uiso 1 1 calc R . .
H34B H 0.6320 1.1210 0.9337 0.134 Uiso 1 1 calc R . .
H34C H 0.6744 1.0543 0.9569 0.134 Uiso 1 1 calc R . .
N1 N 0.70718(14) 0.77482(10) 0.46031(8) 0.0292(4) Uani 1 1 d . . .
N2 N 0.75950(12) 0.91768(10) 0.46470(7) 0.0224(4) Uani 1 1 d . . .
N3 N 0.75470(14) 0.82054(11) 0.58666(8) 0.0279(5) Uani 1 1 d . . .
N4 N 0.58879(12) 0.88270(11) 0.55116(7) 0.0246(4) Uani 1 1 d . . .
O1 O 0.82857(16) 0.83864(13) 0.10773(8) 0.0592(7) Uani 1 1 d . . .
O2 O 0.95173(15) 0.79657(14) 0.14394(8) 0.0572(6) Uani 1 1 d . . .
O3 O 0.5982(2) 0.94247(14) 0.91698(8) 0.0751(8) Uani 1 1 d . . .
O4 O 0.62482(18) 1.04416(13) 0.87980(9) 0.0628(7) Uani 1 1 d . . .
Zn1 Zn 0.699198(17) 0.850569(14) 0.514984(9) 0.02494(7) Uani 1 1 d . . .


_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
C1 N1 1.326(3) . ?
C1 C2 1.406(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.372(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.424(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(4) . ?
C4 N1 1.395(3) . ?
C5 C6 1.393(4) . ?
C5 C10 1.501(3) . ?
C6 N2 1.405(3) . ?
C6 C7 1.428(3) . ?
C7 C8 1.359(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.416(3) . ?
C8 H8 0.9300 . ?
C9 N2 1.347(3) . ?
C9 C9 1.460(4) 3_576 ?
C10 C11 1.374(3) . ?
C10 C15 1.379(4) . ?
C11 C12 1.404(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.366(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.377(4) . ?
C13 C16 1.498(3) . ?
C14 C15 1.383(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O1 1.177(3) . ?
C16 O2 1.349(4) . ?
C17 O2 1.451(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N3 1.319(3) . ?
C18 C19 1.403(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.373(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.421(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.390(3) . ?
C21 N3 1.394(3) . ?
C22 C23 1.418(3) . ?
C22 C27 1.505(3) . ?
C23 N4 1.396(3) . ?
C23 C24 1.410(4) . ?
C24 C25 1.367(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.402(3) . ?
C25 H25 0.9300 . ?
C26 N4 1.355(3) . ?
C26 C26 1.448(4) 4_656 ?
C27 C32 1.376(3) . ?
C27 C28 1.384(4) . ?
C28 C29 1.390(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.391(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.363(4) . ?
C30 C33 1.498(3) . ?
C31 C32 1.381(4) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 O3 1.196(4) . ?
C33 O4 1.326(4) . ?
C34 O4 1.446(4) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
N1 Zn1 1.9800(19) . ?
N2 Zn1 2.0056(19) . ?
N3 Zn1 1.987(2) . ?
N4 Zn1 2.0003(19) . ?

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 C1 C2 112.2(2) . . ?
N1 C1 H1 123.9 . . ?
C2 C1 H1 123.9 . . ?
C3 C2 C1 105.7(2) . . ?
C3 C2 H2 127.1 . . ?
C1 C2 H2 127.1 . . ?
C2 C3 C4 107.5(2) . . ?
C2 C3 H3 126.2 . . ?
C4 C3 H3 126.2 . . ?
C5 C4 N1 124.4(2) . . ?
C5 C4 C3 127.0(2) . . ?
N1 C4 C3 107.9(2) . . ?
C4 C5 C6 127.7(2) . . ?
C4 C5 C10 116.5(2) . . ?
C6 C5 C10 115.7(2) . . ?
C5 C6 N2 126.0(2) . . ?
C5 C6 C7 125.9(2) . . ?
N2 C6 C7 108.0(2) . . ?
C8 C7 C6 107.9(2) . . ?
C8 C7 H7 126.1 . . ?
C6 C7 H7 126.1 . . ?
C7 C8 C9 106.6(2) . . ?
C7 C8 H8 126.7 . . ?
C9 C8 H8 126.7 . . ?
N2 C9 C8 111.17(19) . . ?
N2 C9 C9 122.7(3) . 3_576 ?
C8 C9 C9 125.9(3) . 3_576 ?
C11 C10 C15 119.0(2) . . ?
C11 C10 C5 121.7(2) . . ?
C15 C10 C5 119.3(2) . . ?
C10 C11 C12 120.2(2) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 120.1(2) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 119.8(2) . . ?
C12 C13 C16 118.4(2) . . ?
C14 C13 C16 121.8(3) . . ?
C13 C14 C15 120.1(3) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C10 C15 C14 120.9(2) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
O1 C16 O2 124.2(3) . . ?
O1 C16 C13 125.5(3) . . ?
O2 C16 C13 110.2(2) . . ?
O2 C17 H17A 109.5 . . ?
O2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C18 C19 111.7(2) . . ?
N3 C18 H18 124.1 . . ?
C19 C18 H18 124.1 . . ?
C20 C19 C18 106.6(2) . . ?
C20 C19 H19 126.7 . . ?
C18 C19 H19 126.7 . . ?
C19 C20 C21 106.4(2) . . ?
C19 C20 H20 126.8 . . ?
C21 C20 H20 126.8 . . ?
C22 C21 N3 123.8(2) . . ?
C22 C21 C20 127.7(2) . . ?
N3 C21 C20 108.5(2) . . ?
C21 C22 C23 127.6(2) . . ?
C21 C22 C27 117.7(2) . . ?
C23 C22 C27 114.6(2) . . ?
N4 C23 C24 108.9(2) . . ?
N4 C23 C22 125.8(2) . . ?
C24 C23 C22 125.2(2) . . ?
C25 C24 C23 107.1(2) . . ?
C25 C24 H24 126.4 . . ?
C23 C24 H24 126.4 . . ?
C24 C25 C26 107.3(2) . . ?
C24 C25 H25 126.3 . . ?
C26 C25 H25 126.3 . . ?
N4 C26 C25 110.5(2) . . ?
N4 C26 C26 122.4(3) . 4_656 ?
C25 C26 C26 127.1(3) . 4_656 ?
C32 C27 C28 119.1(2) . . ?
C32 C27 C22 122.6(2) . . ?
C28 C27 C22 118.1(2) . . ?
C27 C28 C29 120.6(2) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C28 C29 C30 119.3(3) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C31 C30 C29 119.7(2) . . ?
C31 C30 C33 119.9(3) . . ?
C29 C30 C33 120.4(3) . . ?
C30 C31 C32 120.9(2) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 H31 119.6 . . ?
C27 C32 C31 120.3(3) . . ?
C27 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
O3 C33 O4 124.0(3) . . ?
O3 C33 C30 123.6(3) . . ?
O4 C33 C30 112.3(3) . . ?
O4 C34 H34A 109.5 . . ?
O4 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O4 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C1 N1 C4 106.6(2) . . ?
C1 N1 Zn1 128.77(16) . . ?
C4 N1 Zn1 124.26(17) . . ?
C9 N2 C6 106.29(19) . . ?
C9 N2 Zn1 131.02(15) . . ?
C6 N2 Zn1 121.17(16) . . ?
C18 N3 C21 106.7(2) . . ?
C18 N3 Zn1 128.14(17) . . ?
C21 N3 Zn1 123.01(16) . . ?
C26 N4 C23 106.18(19) . . ?
C26 N4 Zn1 132.63(14) . . ?
C23 N4 Zn1 121.15(15) . . ?
C16 O2 C17 115.2(3) . . ?
C33 O4 C34 115.8(3) . . ?
N1 Zn1 N3 107.79(8) . . ?
N1 Zn1 N4 124.81(9) . . ?
N3 Zn1 N4 95.29(8) . . ?
N1 Zn1 N2 94.73(8) . . ?
N3 Zn1 N2 120.34(8) . . ?
N4 Zn1 N2 115.77(8) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        30.07
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.064

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 -0.005 898 376 ' '
2 0.095 0.237 0.786 7 0 ' '
3 0.095 0.763 0.214 6 1 ' '
4 0.500 0.500 0.691 898 376 ' '
5 0.404 0.263 0.286 6 1 ' '
6 0.404 0.737 0.714 7 1 ' '
7 0.595 0.263 0.714 6 1 ' '
8 0.595 0.737 0.286 7 0 ' '
9 0.904 0.237 0.214 7 1 ' '
10 0.904 0.763 0.786 6 1 ' '
_platon_squeeze_details          
;
;




#===END


