# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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data_1a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H52 Cl4 N7 O9 Zn2, C2 H6 O, N O3'
_chemical_formula_sum            'C56 H58 Cl4 N8 O13 Zn2'
_chemical_formula_weight         1323.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   13.244(3)
_cell_length_b                   13.505(3)
_cell_length_c                   17.957(4)
_cell_angle_alpha                89.565(3)
_cell_angle_beta                 72.204(2)
_cell_angle_gamma                72.003(3)
_cell_volume                     2895.2(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    4753
_cell_measurement_theta_min      2.394
_cell_measurement_theta_max      24.393

_exptl_crystal_description       block
_exptl_crystal_colour            'yellow green'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1364
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8809
_exptl_absorpt_correction_T_max  0.8993
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'

_exptl_special_details           
; 
The structure was solved by direct methods (Bruker, 2000) and
successive difference Fourier syntheses.
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21458
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10081
_reflns_number_gt                6979
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (BRUKER 2000)'
_computing_cell_refinement       'SMART APEX2 V2011.4-1'
_computing_data_reduction        'SAINT V6.02A (BRUKER 2000)'
_computing_structure_solution    'SHELXTL V6.10 (BRUKER 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0813P)²] 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         10081
_refine_ls_number_parameters     748
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.1397
_refine_ls_wR_factor_gt          0.1277
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.007
_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
Zn1 Zn 0.26985(3) 0.38837(3) 0.09150(2) 0.04304(14) Uani 1 1 d . . .
Zn2 Zn 0.27491(3) 0.53601(3) 0.26952(3) 0.04713(14) Uani 1 1 d . . .
C1 C 0.0352(3) 0.4435(3) 0.19534(19) 0.0378(8) Uani 1 1 d . . .
C2 C -0.0457(3) 0.4158(3) 0.25666(19) 0.0363(8) Uani 1 1 d . . .
C3 C -0.1553(3) 0.4813(3) 0.2858(2) 0.0428(8) Uani 1 1 d . . .
H3 H -0.2080 0.4610 0.3245 0.051 Uiso 1 1 calc R . .
C4 C -0.1854(3) 0.5766(3) 0.2568(2) 0.0448(9) Uani 1 1 d . . .
C5 C -0.1095(3) 0.6075(3) 0.1988(2) 0.0429(8) Uani 1 1 d . . .
H5 H -0.1316 0.6731 0.1810 0.051 Uiso 1 1 calc R . .
C6 C 0.0005(3) 0.5415(3) 0.1665(2) 0.0398(8) Uani 1 1 d . . .
C7 C 0.0716(3) 0.5787(3) 0.1020(2) 0.0458(9) Uani 1 1 d . . .
H7 H 0.0398 0.6435 0.0863 0.055 Uiso 1 1 calc R . .
C8 C 0.2336(3) 0.5712(3) -0.0048(2) 0.0609(11) Uani 1 1 d . . .
H8A H 0.3068 0.5674 -0.0022 0.073 Uiso 1 1 calc R . .
H8B H 0.1923 0.6440 -0.0059 0.073 Uiso 1 1 calc R . .
C9 C 0.2473(4) 0.5085(4) -0.0795(2) 0.0704(13) Uani 1 1 d . . .
H9A H 0.1875 0.5451 -0.1000 0.085 Uiso 1 1 calc R . .
H9B H 0.3175 0.5065 -0.1184 0.085 Uiso 1 1 calc R . .
C10 C 0.2464(4) 0.3985(4) -0.0702(2) 0.0628(12) Uani 1 1 d . . .
H10A H 0.1701 0.3999 -0.0440 0.075 Uiso 1 1 calc R . .
H10B H 0.2710 0.3613 -0.1219 0.075 Uiso 1 1 calc R . .
C11 C 0.4000(3) 0.2596(3) -0.0599(2) 0.0539(10) Uani 1 1 d . . .
H11 H 0.4140 0.2453 -0.1134 0.065 Uiso 1 1 calc R . .
C12 C 0.4739(3) 0.1875(3) -0.0245(2) 0.0475(9) Uani 1 1 d . . .
C13 C 0.5624(3) 0.1078(3) -0.0752(2) 0.0553(10) Uani 1 1 d . . .
H13 H 0.5716 0.1052 -0.1287 0.066 Uiso 1 1 calc R . .
C14 C 0.6347(3) 0.0348(3) -0.0488(2) 0.0539(10) Uani 1 1 d . . .
C15 C 0.6222(3) 0.0347(3) 0.0306(2) 0.0501(9) Uani 1 1 d . . .
H15 H 0.6719 -0.0167 0.0486 0.060 Uiso 1 1 calc R . .
C16 C 0.5355(3) 0.1117(3) 0.0825(2) 0.0411(8) Uani 1 1 d . . .
C17 C 0.4583(3) 0.1923(3) 0.0571(2) 0.0412(8) Uani 1 1 d . . .
C18 C 0.5175(3) 0.1125(3) 0.1683(2) 0.0430(8) Uani 1 1 d . . .
H18A H 0.5715 0.0510 0.1782 0.052 Uiso 1 1 calc R . .
H18B H 0.4432 0.1089 0.1949 0.052 Uiso 1 1 calc R . .
C19 C 0.5136(3) 0.2030(3) 0.2887(2) 0.0441(8) Uani 1 1 d . . .
H19A H 0.4391 0.1999 0.3154 0.053 Uiso 1 1 calc R . .
H19B H 0.5672 0.1391 0.2958 0.053 Uiso 1 1 calc R . .
C20 C 0.5283(3) 0.2933(3) 0.3255(2) 0.0411(8) Uani 1 1 d . . .
C21 C 0.4605(3) 0.3964(3) 0.3193(2) 0.0422(8) Uani 1 1 d . . .
C22 C 0.4769(3) 0.4803(3) 0.3541(2) 0.0483(9) Uani 1 1 d . . .
C23 C 0.5532(3) 0.4612(3) 0.3959(2) 0.0543(10) Uani 1 1 d . . .
H23 H 0.5630 0.5172 0.4192 0.065 Uiso 1 1 calc R . .
C24 C 0.6132(3) 0.3624(4) 0.4029(2) 0.0545(10) Uani 1 1 d . . .
C25 C 0.6026(3) 0.2762(3) 0.3678(2) 0.0476(9) Uani 1 1 d . . .
H25 H 0.6445 0.2086 0.3728 0.057 Uiso 1 1 calc R . .
C26 C 0.4205(4) 0.5891(3) 0.3480(3) 0.0607(11) Uani 1 1 d . . .
H26 H 0.4448 0.6378 0.3675 0.073 Uiso 1 1 calc R . .
C27 C 0.2970(5) 0.7406(4) 0.3195(4) 0.105(2) Uani 1 1 d . . .
H27A H 0.3453 0.7725 0.3342 0.126 Uiso 1 1 calc R . .
H27B H 0.2230 0.7668 0.3581 0.126 Uiso 1 1 calc R . .
C28 C 0.2905(5) 0.7698(5) 0.2405(4) 0.118(2) Uani 1 1 d . . .
H28A H 0.3598 0.7287 0.2014 0.142 Uiso 1 1 calc R . .
H28B H 0.2862 0.8427 0.2376 0.142 Uiso 1 1 calc R . .
C29 C 0.1950(4) 0.7557(4) 0.2187(3) 0.0804(15) Uani 1 1 d . . .
H29A H 0.1350 0.8220 0.2288 0.096 Uiso 1 1 calc R . .
H29B H 0.2197 0.7335 0.1630 0.096 Uiso 1 1 calc R . .
C30 C 0.0506(3) 0.7077(3) 0.3075(2) 0.0545(10) Uani 1 1 d . . .
H30 H 0.0081 0.7764 0.3062 0.065 Uiso 1 1 calc R . .
C31 C -0.0051(3) 0.6449(3) 0.3591(2) 0.0442(9) Uani 1 1 d . . .
C32 C 0.0464(3) 0.5376(3) 0.3634(2) 0.0429(8) Uani 1 1 d . . .
C33 C -0.0198(3) 0.4819(3) 0.41087(19) 0.0413(8) Uani 1 1 d . . .
C34 C -0.1284(3) 0.5321(3) 0.4556(2) 0.0524(10) Uani 1 1 d . . .
H34 H -0.1700 0.4948 0.4878 0.063 Uiso 1 1 calc R . .
C35 C -0.1761(3) 0.6378(3) 0.4530(2) 0.0534(10) Uani 1 1 d . . .
C36 C -0.1173(3) 0.6937(3) 0.4051(2) 0.0503(9) Uani 1 1 d . . .
H36 H -0.1516 0.7645 0.4028 0.060 Uiso 1 1 calc R . .
C37 C 0.0346(3) 0.3672(3) 0.4083(2) 0.0487(9) Uani 1 1 d . . .
H37A H -0.0201 0.3362 0.4386 0.058 Uiso 1 1 calc R . .
H37B H 0.0936 0.3543 0.4321 0.058 Uiso 1 1 calc R . .
C38 C -0.0058(3) 0.3140(3) 0.28901(19) 0.0373(8) Uani 1 1 d . . .
H38A H 0.0249 0.2574 0.2473 0.045 Uiso 1 1 calc R . .
H38B H -0.0682 0.3017 0.3287 0.045 Uiso 1 1 calc R . .
C39 C 0.6368(3) 0.2291(3) 0.1566(2) 0.0427(8) Uani 1 1 d . . .
H39A H 0.6393 0.2363 0.1023 0.051 Uiso 1 1 calc R . .
H39B H 0.6365 0.2948 0.1784 0.051 Uiso 1 1 calc R . .
C40 C 0.7405(3) 0.1436(3) 0.1588(2) 0.0497(9) Uani 1 1 d . . .
H40A H 0.7380 0.0765 0.1420 0.060 Uiso 1 1 calc R . .
H40B H 0.7433 0.1414 0.2121 0.060 Uiso 1 1 calc R . .
C41 C 0.8451(3) 0.1631(3) 0.1049(2) 0.0454(9) Uani 1 1 d . . .
C42 C 0.9000(3) 0.2180(3) 0.1322(2) 0.0564(10) Uani 1 1 d . . .
H42 H 0.8723 0.2450 0.1846 0.068 Uiso 1 1 calc R . .
C43 C 0.9958(4) 0.2343(4) 0.0835(3) 0.0668(12) Uani 1 1 d . . .
H43 H 1.0311 0.2727 0.1031 0.080 Uiso 1 1 calc R . .
C44 C 1.0383(3) 0.1942(3) 0.0071(3) 0.0544(10) Uani 1 1 d . . .
C45 C 0.9834(3) 0.1401(3) -0.0226(2) 0.0578(11) Uani 1 1 d . . .
H45 H 1.0110 0.1138 -0.0751 0.069 Uiso 1 1 calc R . .
C46 C 0.8870(3) 0.1257(3) 0.0270(2) 0.0550(10) Uani 1 1 d . . .
H46 H 0.8497 0.0898 0.0071 0.066 Uiso 1 1 calc R . .
C47 C 0.1745(3) 0.2145(3) 0.3144(3) 0.0586(11) Uani 1 1 d . . .
H47A H 0.2412 0.2285 0.3165 0.070 Uiso 1 1 calc R . .
H47B H 0.1914 0.1817 0.2622 0.070 Uiso 1 1 calc R . .
C48 C 0.1507(4) 0.1365(4) 0.3733(3) 0.0804(15) Uani 1 1 d . . .
H48A H 0.2165 0.0746 0.3604 0.096 Uiso 1 1 calc R . .
H48B H 0.1407 0.1669 0.4249 0.096 Uiso 1 1 calc R . .
C49 C 0.0502(4) 0.1022(3) 0.3789(3) 0.0658(12) Uani 1 1 d . . .
C50 C -0.0307(5) 0.1122(4) 0.4516(3) 0.0788(14) Uani 1 1 d . . .
H50 H -0.0237 0.1419 0.4955 0.095 Uiso 1 1 calc R . .
C51 C -0.1201(5) 0.0788(5) 0.4593(4) 0.0925(17) Uani 1 1 d . . .
H51 H -0.1725 0.0845 0.5086 0.111 Uiso 1 1 calc R . .
C52 C -0.1339(4) 0.0365(4) 0.3943(4) 0.0788(14) Uani 1 1 d . . .
C53 C -0.0558(4) 0.0264(3) 0.3230(3) 0.0768(14) Uani 1 1 d . . .
H53 H -0.0637 -0.0021 0.2789 0.092 Uiso 1 1 calc R . .
C54 C 0.0353(4) 0.0586(3) 0.3162(3) 0.0732(13) Uani 1 1 d . . .
H54 H 0.0889 0.0503 0.2671 0.088 Uiso 1 1 calc R . .
C55 C 0.4749(7) 0.8820(6) 0.4375(5) 0.157(3) Uani 1 1 d D . .
H55A H 0.4592 0.8200 0.4261 0.235 Uiso 1 1 calc R . .
H55B H 0.4442 0.9024 0.4930 0.235 Uiso 1 1 calc R . .
H55C H 0.5544 0.8682 0.4209 0.235 Uiso 1 1 calc R . .
C56 C 0.4250(7) 0.9652(8) 0.3962(7) 0.198(5) Uani 1 1 d D . .
H56A H 0.4483 1.0249 0.4032 0.237 Uiso 1 1 calc R . .
H56B H 0.3442 0.9863 0.4192 0.237 Uiso 1 1 calc R . .
Cl1 Cl -0.32171(9) 0.66274(9) 0.29613(7) 0.0717(3) Uani 1 1 d . . .
Cl2 Cl 0.74549(11) -0.06335(10) -0.11380(8) 0.0888(4) Uani 1 1 d . . .
Cl3 Cl -0.31408(10) 0.69974(12) 0.51158(7) 0.0893(4) Uani 1 1 d . . .
Cl4 Cl 0.70756(10) 0.33986(11) 0.45610(7) 0.0758(3) Uani 1 1 d . . .
N1 N 0.1734(3) 0.5301(2) 0.06534(18) 0.0483(8) Uani 1 1 d . . .
N2 N 0.3174(3) 0.3411(3) -0.02557(17) 0.0493(8) Uani 1 1 d . . .
N3 N 0.1527(3) 0.6781(2) 0.2634(2) 0.0566(9) Uani 1 1 d . . .
N4 N 0.3415(3) 0.6257(3) 0.3190(2) 0.0646(10) Uani 1 1 d . . .
N5 N 0.0835(2) 0.3166(2) 0.32507(16) 0.0405(7) Uani 1 1 d . . .
N6 N 0.5291(2) 0.2087(2) 0.20189(16) 0.0384(6) Uani 1 1 d . . .
N7 N 0.4363(3) 0.4794(3) 0.1153(2) 0.0647(10) Uani 1 1 d . . .
N8 N 0.7583(5) 0.9021(3) 0.2328(3) 0.0799(12) Uani 1 1 d . . .
O1 O 0.13707(19) 0.37692(18) 0.17192(13) 0.0451(6) Uani 1 1 d . . .
H1 H 0.1476 0.3158 0.1970 0.054 Uiso 1 1 d R . .
O2 O 0.3803(2) 0.26229(18) 0.11085(13) 0.0443(6) Uani 1 1 d . . .
O3 O 0.1499(2) 0.48526(18) 0.32468(15) 0.0485(6) Uani 1 1 d . . .
H3A H 0.1676 0.4129 0.3227 0.058 Uiso 1 1 calc R . .
O4 O 0.3899(2) 0.40449(19) 0.28099(15) 0.0501(6) Uani 1 1 d . . .
O5 O -0.2264(4) 0.0028(4) 0.4070(3) 0.1228(15) Uani 1 1 d . . .
H5A H -0.2234 -0.0256 0.3658 0.184 Uiso 1 1 d R . .
O6 O 1.1332(3) 0.2113(3) -0.0385(2) 0.0854(10) Uani 1 1 d . . .
H6 H 1.1568 0.1759 -0.0808 0.128 Uiso 1 1 d R . .
O7 O 0.3300(2) 0.4889(2) 0.14912(15) 0.0514(6) Uani 1 1 d . . .
O8 O 0.4859(3) 0.4203(3) 0.0551(2) 0.0875(11) Uani 1 1 d . . .
O9 O 0.4782(3) 0.5287(4) 0.1457(2) 0.1116(15) Uani 1 1 d . . .
O10 O 0.7193(4) 0.8837(3) 0.1836(3) 0.1121(14) Uani 1 1 d . . .
O11 O 0.8600(4) 0.8699(3) 0.2202(2) 0.0995(12) Uani 1 1 d . . .
O12 O 0.6957(4) 0.9555(3) 0.2943(3) 0.1129(14) Uani 1 1 d . . .
O13 O 0.4548(5) 0.9364(6) 0.3128(4) 0.183(3) Uani 1 1 d . . .
H13A H 0.5338 0.8958 0.2945 0.275 Uiso 1 1 d R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.953(2) . ?
Zn1 O2 1.980(2) . ?
Zn1 N2 2.046(3) . ?
Zn1 N1 2.088(3) . ?
Zn1 O7 2.177(3) . ?
Zn2 O3 1.970(2) . ?
Zn2 O4 2.008(2) . ?
Zn2 N4 2.047(3) . ?
Zn2 O7 2.093(3) . ?
Zn2 N3 2.121(3) . ?
C1 O1 1.309(4) . ?
C1 C6 1.411(5) . ?
C1 C2 1.421(5) . ?
C2 C3 1.383(5) . ?
C2 C38 1.494(4) . ?
C3 C4 1.373(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(5) . ?
C4 Cl1 1.746(4) . ?
C5 C6 1.393(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.448(5) . ?
C7 N1 1.265(5) . ?
C7 H7 0.9300 . ?
C8 N1 1.476(5) . ?
C8 C9 1.525(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.497(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.459(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.281(5) . ?
C11 C12 1.446(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.394(5) . ?
C12 C17 1.416(5) . ?
C13 C14 1.342(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.384(5) . ?
C14 Cl2 1.746(4) . ?
C15 C16 1.376(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.424(5) . ?
C16 C18 1.484(5) . ?
C17 O2 1.301(4) . ?
C18 N6 1.505(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.482(5) . ?
C19 N6 1.514(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C25 1.384(5) . ?
C20 C21 1.429(5) . ?
C21 O4 1.300(4) . ?
C21 C22 1.402(5) . ?
C22 C23 1.397(5) . ?
C22 C26 1.449(6) . ?
C23 C24 1.353(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.392(6) . ?
C24 Cl4 1.749(4) . ?
C25 H25 0.9300 . ?
C26 N4 1.272(5) . ?
C26 H26 0.9300 . ?
C27 N4 1.479(6) . ?
C27 C28 1.490(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.498(8) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 N3 1.460(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N3 1.277(5) . ?
C30 C31 1.441(5) . ?
C30 H30 0.9300 . ?
C31 C36 1.407(5) . ?
C31 C32 1.411(5) . ?
C32 O3 1.299(4) . ?
C32 C33 1.415(5) . ?
C33 C34 1.368(5) . ?
C33 C37 1.487(5) . ?
C34 C35 1.378(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.364(6) . ?
C35 Cl3 1.744(4) . ?
C36 H36 0.9300 . ?
C37 N5 1.508(5) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 N5 1.521(4) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.508(5) . ?
C39 N6 1.517(4) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.525(5) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.368(5) . ?
C41 C46 1.372(5) . ?
C42 C43 1.383(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.358(6) . ?
C43 H43 0.9300 . ?
C44 O6 1.360(5) . ?
C44 C45 1.383(6) . ?
C45 C46 1.386(5) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C47 N5 1.492(5) . ?
C47 C48 1.520(6) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 C49 1.516(6) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 C54 1.367(6) . ?
C49 C50 1.389(7) . ?
C50 C51 1.361(7) . ?
C50 H50 0.9300 . ?
C51 C52 1.387(7) . ?
C51 H51 0.9300 . ?
C52 C53 1.355(7) . ?
C52 O5 1.391(6) . ?
C53 C54 1.376(6) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
C55 C56 1.441(7) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 O13 1.449(12) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
N7 O9 1.211(5) . ?
N7 O8 1.221(5) . ?
N7 O7 1.318(4) . ?
N8 O10 1.212(6) . ?
N8 O11 1.228(6) . ?
N8 O12 1.229(5) . ?
O1 H1 0.9300 . ?
O3 H3A 0.9300 . ?
O5 H5A 0.8200 . ?
O6 H6 0.8200 . ?
O13 H13A 0.9700 . ?

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
O1 Zn1 O2 97.61(10) . . ?
O1 Zn1 N2 125.58(11) . . ?
O2 Zn1 N2 92.66(11) . . ?
O1 Zn1 N1 89.97(11) . . ?
O2 Zn1 N1 171.40(11) . . ?
N2 Zn1 N1 86.16(12) . . ?
O1 Zn1 O7 104.75(10) . . ?
O2 Zn1 O7 90.72(10) . . ?
N2 Zn1 O7 128.49(11) . . ?
N1 Zn1 O7 83.39(11) . . ?
O3 Zn2 O4 92.50(10) . . ?
O3 Zn2 N4 126.45(13) . . ?
O4 Zn2 N4 91.11(12) . . ?
O3 Zn2 O7 110.14(11) . . ?
O4 Zn2 O7 87.76(10) . . ?
N4 Zn2 O7 123.39(13) . . ?
O3 Zn2 N3 87.29(11) . . ?
O4 Zn2 N3 176.94(12) . . ?
N4 Zn2 N3 86.57(14) . . ?
O7 Zn2 N3 95.19(12) . . ?
O1 C1 C6 125.3(3) . . ?
O1 C1 C2 117.0(3) . . ?
C6 C1 C2 117.6(3) . . ?
C3 C2 C1 121.3(3) . . ?
C3 C2 C38 121.9(3) . . ?
C1 C2 C38 116.7(3) . . ?
C4 C3 C2 119.2(3) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C4 C3 121.4(3) . . ?
C5 C4 Cl1 118.7(3) . . ?
C3 C4 Cl1 119.8(3) . . ?
C4 C5 C6 120.5(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 C7 116.0(3) . . ?
C1 C6 C7 124.1(3) . . ?
N1 C7 C6 125.3(3) . . ?
N1 C7 H7 117.3 . . ?
C6 C7 H7 117.3 . . ?
N1 C8 C9 110.6(3) . . ?
N1 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C8 115.4(3) . . ?
C10 C9 H9A 108.4 . . ?
C8 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
C8 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
N2 C10 C9 113.8(4) . . ?
N2 C10 H10A 108.8 . . ?
C9 C10 H10A 108.8 . . ?
N2 C10 H10B 108.8 . . ?
C9 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N2 C11 C12 127.0(4) . . ?
N2 C11 H11 116.5 . . ?
C12 C11 H11 116.5 . . ?
C13 C12 C17 119.8(4) . . ?
C13 C12 C11 116.4(4) . . ?
C17 C12 C11 123.7(3) . . ?
C14 C13 C12 121.7(4) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C13 C14 C15 120.8(4) . . ?
C13 C14 Cl2 120.6(3) . . ?
C15 C14 Cl2 118.5(3) . . ?
C16 C15 C14 119.2(4) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 122.0(3) . . ?
C15 C16 C18 120.8(3) . . ?
C17 C16 C18 117.2(3) . . ?
O2 C17 C12 126.5(3) . . ?
O2 C17 C16 117.2(3) . . ?
C12 C17 C16 116.4(3) . . ?
C16 C18 N6 112.6(3) . . ?
C16 C18 H18A 109.1 . . ?
N6 C18 H18A 109.1 . . ?
C16 C18 H18B 109.1 . . ?
N6 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 N6 113.1(3) . . ?
C20 C19 H19A 109.0 . . ?
N6 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
N6 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C25 C20 C21 121.6(3) . . ?
C25 C20 C19 119.7(3) . . ?
C21 C20 C19 118.6(3) . . ?
O4 C21 C22 125.5(3) . . ?
O4 C21 C20 117.2(3) . . ?
C22 C21 C20 117.3(3) . . ?
C23 C22 C21 120.0(4) . . ?
C23 C22 C26 116.3(4) . . ?
C21 C22 C26 123.7(3) . . ?
C24 C23 C22 121.0(4) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 121.4(4) . . ?
C23 C24 Cl4 120.4(3) . . ?
C25 C24 Cl4 118.1(3) . . ?
C20 C25 C24 118.5(4) . . ?
C20 C25 H25 120.8 . . ?
C24 C25 H25 120.8 . . ?
N4 C26 C22 127.6(4) . . ?
N4 C26 H26 116.2 . . ?
C22 C26 H26 116.2 . . ?
N4 C27 C28 110.6(5) . . ?
N4 C27 H27A 109.5 . . ?
C28 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C27 C28 C29 116.6(5) . . ?
C27 C28 H28A 108.1 . . ?
C29 C28 H28A 108.1 . . ?
C27 C28 H28B 108.1 . . ?
C29 C28 H28B 108.1 . . ?
H28A C28 H28B 107.3 . . ?
N3 C29 C28 111.3(4) . . ?
N3 C29 H29A 109.4 . . ?
C28 C29 H29A 109.4 . . ?
N3 C29 H29B 109.4 . . ?
C28 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
N3 C30 C31 126.3(3) . . ?
N3 C30 H30 116.8 . . ?
C31 C30 H30 116.8 . . ?
C36 C31 C32 119.3(3) . . ?
C36 C31 C30 117.4(3) . . ?
C32 C31 C30 123.2(3) . . ?
O3 C32 C31 124.5(3) . . ?
O3 C32 C33 117.4(3) . . ?
C31 C32 C33 118.1(3) . . ?
C34 C33 C32 121.0(3) . . ?
C34 C33 C37 122.6(3) . . ?
C32 C33 C37 116.4(3) . . ?
C33 C34 C35 120.1(4) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C36 C35 C34 121.0(4) . . ?
C36 C35 Cl3 120.0(3) . . ?
C34 C35 Cl3 119.0(3) . . ?
C35 C36 C31 120.4(4) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C33 C37 N5 111.2(3) . . ?
C33 C37 H37A 109.4 . . ?
N5 C37 H37A 109.4 . . ?
C33 C37 H37B 109.4 . . ?
N5 C37 H37B 109.4 . . ?
H37A C37 H37B 108.0 . . ?
C2 C38 N5 109.7(3) . . ?
C2 C38 H38A 109.7 . . ?
N5 C38 H38A 109.7 . . ?
C2 C38 H38B 109.7 . . ?
N5 C38 H38B 109.7 . . ?
H38A C38 H38B 108.2 . . ?
C40 C39 N6 113.1(3) . . ?
C40 C39 H39A 109.0 . . ?
N6 C39 H39A 108.9 . . ?
C40 C39 H39B 108.9 . . ?
N6 C39 H39B 109.0 . . ?
H39A C39 H39B 107.8 . . ?
C39 C40 C41 110.3(3) . . ?
C39 C40 H40A 109.6 . . ?
C41 C40 H40A 109.6 . . ?
C39 C40 H40B 109.6 . . ?
C41 C40 H40B 109.6 . . ?
H40A C40 H40B 108.1 . . ?
C42 C41 C46 118.0(4) . . ?
C42 C41 C40 121.6(4) . . ?
C46 C41 C40 120.4(3) . . ?
C41 C42 C43 121.5(4) . . ?
C41 C42 H42 119.3 . . ?
C43 C42 H42 119.3 . . ?
C44 C43 C42 120.0(4) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 O6 118.0(4) . . ?
C43 C44 C45 119.8(4) . . ?
O6 C44 C45 122.2(4) . . ?
C44 C45 C46 119.2(4) . . ?
C44 C45 H45 120.4 . . ?
C46 C45 H45 120.4 . . ?
C41 C46 C45 121.5(4) . . ?
C41 C46 H46 119.3 . . ?
C45 C46 H46 119.3 . . ?
N5 C47 C48 116.5(4) . . ?
N5 C47 H47A 108.2 . . ?
C48 C47 H47A 108.2 . . ?
N5 C47 H47B 108.2 . . ?
C48 C47 H47B 108.2 . . ?
H47A C47 H47B 107.3 . . ?
C49 C48 C47 117.0(4) . . ?
C49 C48 H48A 108.1 . . ?
C47 C48 H48A 108.1 . . ?
C49 C48 H48B 108.1 . . ?
C47 C48 H48B 108.1 . . ?
H48A C48 H48B 107.3 . . ?
C54 C49 C50 117.2(5) . . ?
C54 C49 C48 123.7(5) . . ?
C50 C49 C48 119.1(5) . . ?
C51 C50 C49 120.7(5) . . ?
C51 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C50 C51 C52 120.7(5) . . ?
C50 C51 H51 119.6 . . ?
C52 C51 H51 119.6 . . ?
C53 C52 C51 119.3(5) . . ?
C53 C52 O5 123.3(6) . . ?
C51 C52 O5 117.4(5) . . ?
C52 C53 C54 119.5(5) . . ?
C52 C53 H53 120.3 . . ?
C54 C53 H53 120.3 . . ?
C49 C54 C53 122.6(5) . . ?
C49 C54 H54 118.7 . . ?
C53 C54 H54 118.7 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C55 C56 O13 113.5(9) . . ?
C55 C56 H56A 108.9 . . ?
O13 C56 H56A 108.9 . . ?
C55 C56 H56B 108.9 . . ?
O13 C56 H56B 108.9 . . ?
H56A C56 H56B 107.7 . . ?
C7 N1 C8 120.1(3) . . ?
C7 N1 Zn1 126.1(2) . . ?
C8 N1 Zn1 113.8(2) . . ?
C11 N2 C10 118.6(3) . . ?
C11 N2 Zn1 123.8(3) . . ?
C10 N2 Zn1 117.4(3) . . ?
C30 N3 C29 117.8(4) . . ?
C30 N3 Zn2 124.5(3) . . ?
C29 N3 Zn2 116.2(3) . . ?
C26 N4 C27 117.7(4) . . ?
C26 N4 Zn2 124.3(3) . . ?
C27 N4 Zn2 118.0(3) . . ?
C47 N5 C37 113.8(3) . . ?
C47 N5 C38 114.1(3) . . ?
C37 N5 C38 112.7(3) . . ?
C18 N6 C19 109.9(2) . . ?
C18 N6 C39 112.9(3) . . ?
C19 N6 C39 113.0(3) . . ?
O9 N7 O8 124.7(4) . . ?
O9 N7 O7 118.5(4) . . ?
O8 N7 O7 116.8(4) . . ?
O10 N8 O11 120.2(5) . . ?
O10 N8 O12 119.6(6) . . ?
O11 N8 O12 120.2(6) . . ?
C1 O1 Zn1 128.9(2) . . ?
C1 O1 H1 115.5 . . ?
Zn1 O1 H1 115.6 . . ?
C17 O2 Zn1 125.7(2) . . ?
C32 O3 Zn2 129.8(2) . . ?
C32 O3 H3A 115.1 . . ?
Zn2 O3 H3A 115.1 . . ?
C21 O4 Zn2 126.9(2) . . ?
C52 O5 H5A 109.4 . . ?
C44 O6 H6 109.5 . . ?
N7 O7 Zn2 112.5(2) . . ?
N7 O7 Zn1 114.1(3) . . ?
Zn2 O7 Zn1 126.25(12) . . ?
C56 O13 H13A 107.2 . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.066
_database_code_depnum_ccdc_archive 'CCDC 955028'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H52 Cl4 N7 O7 Zn2, C H4 O, N O3'
_chemical_formula_sum            'C55 H56 Cl4 N8 O11 Zn2'
_chemical_formula_weight         1277.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   13.6893(9)
_cell_length_b                   14.9431(10)
_cell_length_c                   15.5399(10)
_cell_angle_alpha                105.0660(10)
_cell_angle_beta                 107.2770(10)
_cell_angle_gamma                93.0690(10)
_cell_volume                     2901.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    4493
_cell_measurement_theta_min      2.269
_cell_measurement_theta_max      23.921

_exptl_crystal_description       block
_exptl_crystal_colour            'yellow green'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_exptl_absorpt_coefficient_mu    1.076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5740
_exptl_absorpt_correction_T_max  0.5740
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'

_exptl_special_details           
; 
The structure was solved by direct methods (Bruker, 2000) and
successive difference Fourier syntheses.
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            16241
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10158
_reflns_number_gt                7196
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (BRUKER 2000)'
_computing_cell_refinement       'SMART APEX2 V2011.4-1'
_computing_data_reduction        'SAINT V6.02A (BRUKER 2000)'
_computing_structure_solution    'SHELXTL V6.10 (BRUKER 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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. There are three large Q 
 peaks after the final refinement, two of them are very close to the each 
 heavy Zn(II) ion (Zn1-Q2 = 0.866 Ang and Zn2-Q3 = 0.870 Ang). However, 
 the largest Q1 peak is near to three atoms (one hydrogen atom of phenolic 
 unit, the central nitrogen atom and the bridging oxygen atom of nitrate 
 anion) (H4A-Q1 = 1.305 Ang, N7-Q1 = 1.662 Ang and O5-Q1 = 1.743 Ang), 
 so it seems that no chemically reasonable atom can be assigned here in 
 this special case, and a disorder model for the bridging nitrate anion 
 is unsuccessful too.
;

_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)+(0.0905P)²+9.8252P] 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         10158
_refine_ls_number_parameters     721
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0794
_refine_ls_wR_factor_ref         0.2098
_refine_ls_wR_factor_gt          0.1966
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_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
Zn1 Zn 0.70662(5) 0.33129(4) 0.40534(5) 0.0548(2) Uani 1 1 d . . .
Zn2 Zn 0.95314(5) 0.22651(5) 0.48070(5) 0.0553(2) Uani 1 1 d . . .
C1 C 0.6021(4) 0.1378(4) 0.3137(4) 0.0470(13) Uani 1 1 d . . .
C2 C 0.5502(4) 0.0577(4) 0.3233(4) 0.0500(13) Uani 1 1 d . . .
C3 C 0.4819(5) -0.0091(4) 0.2460(5) 0.0583(15) Uani 1 1 d . . .
H3 H 0.4479 -0.0607 0.2533 0.070 Uiso 1 1 calc R . .
C4 C 0.4657(5) 0.0030(5) 0.1574(5) 0.0654(17) Uani 1 1 d . . .
C5 C 0.5191(5) 0.0765(5) 0.1455(4) 0.0619(16) Uani 1 1 d . . .
H5 H 0.5098 0.0806 0.0850 0.074 Uiso 1 1 calc R . .
C6 C 0.5862(5) 0.1444(4) 0.2213(4) 0.0526(14) Uani 1 1 d . . .
C7 C 0.5780(4) 0.0454(4) 0.4199(4) 0.0539(14) Uani 1 1 d . . .
H7A H 0.5365 -0.0102 0.4180 0.065 Uiso 1 1 calc R . .
H7B H 0.5627 0.0989 0.4622 0.065 Uiso 1 1 calc R . .
C8 C 0.7212(5) -0.0447(4) 0.3946(4) 0.0568(15) Uani 1 1 d . . .
H8A H 0.6646 -0.0961 0.3687 0.068 Uiso 1 1 calc R . .
H8B H 0.7802 -0.0655 0.4329 0.068 Uiso 1 1 calc R . .
C9 C 0.7484(4) -0.0224(4) 0.3148(4) 0.0518(13) Uani 1 1 d . . .
C10 C 0.8249(4) 0.0557(4) 0.3375(4) 0.0498(13) Uani 1 1 d . . .
C11 C 0.8511(5) 0.0769(4) 0.2628(5) 0.0581(15) Uani 1 1 d . . .
C12 C 0.8047(6) 0.0187(5) 0.1706(5) 0.0679(17) Uani 1 1 d . . .
H12 H 0.8225 0.0323 0.1216 0.081 Uiso 1 1 calc R . .
C13 C 0.7344(6) -0.0570(5) 0.1516(5) 0.0678(18) Uani 1 1 d . . .
C14 C 0.7046(5) -0.0783(4) 0.2240(5) 0.0601(15) Uani 1 1 d . . .
H14 H 0.6556 -0.1299 0.2104 0.072 Uiso 1 1 calc R . .
C15 C 0.9282(6) 0.1552(5) 0.2760(5) 0.0654(17) Uani 1 1 d . . .
H15 H 0.9443 0.1595 0.2230 0.078 Uiso 1 1 calc R . .
C16 C 1.0518(7) 0.2906(5) 0.3523(6) 0.088(2) Uani 1 1 d . . .
H16A H 1.0570 0.2790 0.2896 0.106 Uiso 1 1 calc R . .
H16B H 1.0281 0.3509 0.3683 0.106 Uiso 1 1 calc R . .
C17 C 1.1548(7) 0.2942(6) 0.4196(8) 0.105(3) Uani 1 1 d . . .
H17A H 1.1732 0.3560 0.4645 0.126 Uiso 1 1 calc R . .
H17B H 1.2037 0.2881 0.3850 0.126 Uiso 1 1 calc R . .
C18 C 1.1707(6) 0.2240(5) 0.4743(6) 0.084(2) Uani 1 1 d . . .
H18A H 1.1502 0.1614 0.4310 0.101 Uiso 1 1 calc R . .
H18B H 1.2435 0.2303 0.5096 0.101 Uiso 1 1 calc R . .
C19 C 1.1582(5) 0.2592(4) 0.6285(6) 0.075(2) Uani 1 1 d . . .
H19 H 1.2300 0.2661 0.6468 0.090 Uiso 1 1 calc R . .
C20 C 1.1129(5) 0.2746(4) 0.7032(5) 0.0695(18) Uani 1 1 d . . .
C21 C 1.0052(5) 0.2716(4) 0.6886(5) 0.0574(15) Uani 1 1 d . . .
C22 C 0.9741(6) 0.2939(4) 0.7702(5) 0.0657(17) Uani 1 1 d . . .
C23 C 1.0457(7) 0.3166(5) 0.8604(5) 0.082(2) Uani 1 1 d . . .
H23 H 1.0236 0.3286 0.9129 0.099 Uiso 1 1 calc R . .
C24 C 1.1502(8) 0.3209(6) 0.8712(6) 0.097(3) Uani 1 1 d . . .
C25 C 1.1826(6) 0.3010(5) 0.7955(6) 0.086(2) Uani 1 1 d . . .
H25 H 1.2531 0.3049 0.8045 0.104 Uiso 1 1 calc R . .
C26 C 0.8614(6) 0.2972(4) 0.7576(5) 0.0669(17) Uani 1 1 d . . .
H26A H 0.8508 0.3086 0.8183 0.080 Uiso 1 1 calc R . .
H26B H 0.8221 0.2371 0.7177 0.080 Uiso 1 1 calc R . .
C27 C 0.7127(5) 0.3835(5) 0.7150(5) 0.0692(18) Uani 1 1 d . . .
H27A H 0.6683 0.3243 0.6812 0.083 Uiso 1 1 calc R . .
H27B H 0.7123 0.4002 0.7796 0.083 Uiso 1 1 calc R . .
C28 C 0.6727(5) 0.4563(5) 0.6712(5) 0.0662(18) Uani 1 1 d . . .
C29 C 0.6668(4) 0.4443(4) 0.5779(5) 0.0573(16) Uani 1 1 d . . .
C30 C 0.6340(5) 0.5167(4) 0.5369(5) 0.0669(18) Uani 1 1 d . . .
C31 C 0.6075(5) 0.5966(5) 0.5900(7) 0.076(2) Uani 1 1 d . . .
H31 H 0.5859 0.6440 0.5633 0.092 Uiso 1 1 calc R . .
C32 C 0.6132(5) 0.6052(5) 0.6806(7) 0.087(3) Uani 1 1 d . . .
C33 C 0.6449(5) 0.5377(5) 0.7221(6) 0.079(2) Uani 1 1 d . . .
H33 H 0.6483 0.5453 0.7842 0.095 Uiso 1 1 calc R . .
C34 C 0.6282(5) 0.5160(4) 0.4435(6) 0.0695(19) Uani 1 1 d . . .
H34 H 0.6052 0.5676 0.4249 0.083 Uiso 1 1 calc R . .
C35 C 0.6453(7) 0.4690(5) 0.2924(6) 0.086(2) Uani 1 1 d . . .
H35A H 0.6301 0.5320 0.2944 0.103 Uiso 1 1 calc R . .
H35B H 0.5898 0.4254 0.2422 0.103 Uiso 1 1 calc R . .
C36 C 0.7462(7) 0.4571(5) 0.2728(6) 0.090(2) Uani 1 1 d . . .
H36A H 0.8029 0.4809 0.3314 0.108 Uiso 1 1 calc R . .
H36B H 0.7532 0.4940 0.2314 0.108 Uiso 1 1 calc R . .
C37 C 0.7537(7) 0.3543(5) 0.2268(6) 0.083(2) Uani 1 1 d . . .
H37A H 0.7212 0.3391 0.1592 0.099 Uiso 1 1 calc R . .
H37B H 0.8259 0.3461 0.2390 0.099 Uiso 1 1 calc R . .
C38 C 0.6434(5) 0.2186(5) 0.2026(5) 0.0609(16) Uani 1 1 d . . .
H38 H 0.6353 0.2134 0.1399 0.073 Uiso 1 1 calc R . .
C39 C 0.7131(6) 0.0256(6) 0.5558(5) 0.080(2) Uani 1 1 d . . .
H39A H 0.6833 0.0731 0.5915 0.096 Uiso 1 1 calc R . .
H39B H 0.6790 -0.0350 0.5508 0.096 Uiso 1 1 calc R . .
C40 C 0.8224(6) 0.0332(5) 0.6078(5) 0.082(2) Uani 1 1 d . . .
H40A H 0.8561 0.0948 0.6152 0.098 Uiso 1 1 calc R . .
H40B H 0.8530 -0.0126 0.5710 0.098 Uiso 1 1 calc R . .
C41 C 0.8440(7) 0.0180(5) 0.7067(5) 0.0777(19) Uani 1 1 d U . .
C42 C 0.7687(7) -0.0408(7) 0.7201(6) 0.097(2) Uani 1 1 d U . .
H42 H 0.7066 -0.0670 0.6724 0.116 Uiso 1 1 calc R . .
C43 C 0.7920(9) -0.0586(8) 0.8115(7) 0.113(3) Uani 1 1 d . . .
H43 H 0.7461 -0.0975 0.8241 0.136 Uiso 1 1 calc R . .
C44 C 0.8838(9) -0.0157(8) 0.8776(6) 0.102(3) Uani 1 1 d . . .
H44 H 0.9009 -0.0234 0.9376 0.123 Uiso 1 1 calc R . .
C45 C 0.9517(9) 0.0393(7) 0.8554(8) 0.111(3) Uani 1 1 d . . .
H45 H 1.0148 0.0668 0.9009 0.133 Uiso 1 1 calc R . .
C46 C 0.9311(8) 0.0537(6) 0.7745(7) 0.096(3) Uani 1 1 d . . .
H46 H 0.9800 0.0911 0.7636 0.115 Uiso 1 1 calc R . .
C47 C 0.8942(5) 0.4662(4) 0.7562(4) 0.0582(15) Uani 1 1 d . . .
H47A H 0.9615 0.4561 0.7500 0.070 Uiso 1 1 calc R . .
H47B H 0.8672 0.5096 0.7213 0.070 Uiso 1 1 calc R . .
C48 C 0.9060(6) 0.5084(5) 0.8578(5) 0.0738(19) Uani 1 1 d . . .
H48A H 0.9296 0.4640 0.8925 0.089 Uiso 1 1 calc R . .
H48B H 0.8397 0.5225 0.8641 0.089 Uiso 1 1 calc R . .
C49 C 0.9840(6) 0.5983(5) 0.8987(5) 0.0703(18) Uani 1 1 d . . .
C50 C 1.0869(7) 0.5966(7) 0.9415(5) 0.091(2) Uani 1 1 d . . .
H50 H 1.1112 0.5398 0.9425 0.109 Uiso 1 1 calc R . .
C51 C 1.1562(8) 0.6814(10) 0.9842(6) 0.115(4) Uani 1 1 d . . .
H51 H 1.2256 0.6809 1.0152 0.137 Uiso 1 1 calc R . .
C52 C 1.1204(12) 0.7621(9) 0.9794(9) 0.127(5) Uani 1 1 d . . .
H52 H 1.1660 0.8177 1.0071 0.153 Uiso 1 1 calc R . .
C53 C 1.0197(13) 0.7649(7) 0.9352(8) 0.130(4) Uani 1 1 d . . .
H53 H 0.9965 0.8219 0.9332 0.156 Uiso 1 1 calc R . .
C54 C 0.9518(8) 0.6822(5) 0.8931(6) 0.100(3) Uani 1 1 d . . .
H54 H 0.8831 0.6838 0.8606 0.120 Uiso 1 1 calc R . .
Cl1 Cl 0.37828(18) -0.08196(16) 0.06043(14) 0.0972(7) Uani 1 1 d . . .
Cl2 Cl 0.6798(2) -0.13050(16) 0.03734(14) 0.1048(7) Uani 1 1 d . . .
Cl3 Cl 1.2402(3) 0.3595(3) 0.98412(19) 0.1529(14) Uani 1 1 d . . .
Cl4 Cl 0.5821(2) 0.70751(16) 0.7464(2) 0.1270(10) Uani 1 1 d . . .
N1 N 0.6905(4) 0.0364(3) 0.4564(3) 0.0508(11) Uani 1 1 d . . .
N2 N 0.9749(4) 0.2171(4) 0.3519(4) 0.0649(14) Uani 1 1 d . . .
N3 N 1.1103(4) 0.2370(4) 0.5398(5) 0.0695(15) Uani 1 1 d . . .
N4 N 0.8221(4) 0.3734(3) 0.7136(4) 0.0572(12) Uani 1 1 d . . .
N5 N 0.6513(4) 0.4520(4) 0.3818(4) 0.0683(15) Uani 1 1 d . . .
N6 N 0.7032(4) 0.2894(4) 0.2636(4) 0.0600(13) Uani 1 1 d . . .
N7 N 0.9191(4) 0.4213(4) 0.5255(4) 0.0601(13) Uani 1 1 d . . .
N8 N 0.4722(6) 0.2251(5) 0.6029(9) 0.112(3) Uani 1 1 d . . .
O1 O 0.6636(3) 0.1977(3) 0.3889(3) 0.0542(10) Uani 1 1 d . . .
O2 O 0.8660(3) 0.1038(3) 0.4264(3) 0.0548(10) Uani 1 1 d . . .
H2A H 0.8079 0.1114 0.4500 0.082 Uiso 1 1 d R . .
O3 O 0.9335(3) 0.2516(3) 0.6077(3) 0.0594(10) Uani 1 1 d . . .
O4 O 0.6938(3) 0.3674(3) 0.5332(3) 0.0629(11) Uani 1 1 d . . .
H4A H 0.7612 0.3635 0.5747 0.094 Uiso 1 1 d R . .
O5 O 0.8701(3) 0.3422(3) 0.4601(3) 0.0571(10) Uani 1 1 d . . .
O6 O 0.8722(4) 0.4879(3) 0.5390(4) 0.0838(15) Uani 1 1 d . . .
O7 O 1.0102(4) 0.4243(4) 0.5712(4) 0.0837(15) Uani 1 1 d . . .
O8 O 0.4416(8) 0.2887(7) 0.6496(8) 0.187(5) Uani 1 1 d . . .
O9 O 0.5402(6) 0.1846(4) 0.6384(6) 0.124(2) Uani 1 1 d . . .
O10 O 0.4306(7) 0.2016(7) 0.5145(9) 0.178(4) Uani 1 1 d . . .
O11 O 0.5750(18) 0.3590(19) 0.8797(17) 0.443(18) Uani 1 1 d . . .
H11A H 0.5801 0.3058 0.8462 0.664 Uiso 1 1 d R . .
C55 C 0.505(2) 0.332(2) 0.912(4) 0.58(5) Uani 1 1 d . . .
H55A H 0.5263 0.2850 0.9422 0.873 Uiso 1 1 d R . .
H55B H 0.4976 0.3868 0.9569 0.873 Uiso 1 1 d R . .
H55C H 0.4400 0.3087 0.8626 0.873 Uiso 1 1 d R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.980(4) . ?
Zn1 O4 1.983(4) . ?
Zn1 N5 2.070(5) . ?
Zn1 N6 2.114(5) . ?
Zn1 O5 2.126(4) . ?
Zn2 O2 1.965(4) . ?
Zn2 O3 2.012(4) . ?
Zn2 N3 2.053(6) . ?
Zn2 N2 2.080(5) . ?
Zn2 O5 2.160(4) . ?
C1 O1 1.291(6) . ?
C1 C6 1.417(8) . ?
C1 C2 1.423(8) . ?
C2 C3 1.386(8) . ?
C2 C7 1.498(8) . ?
C3 C4 1.390(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.369(9) . ?
C4 Cl1 1.756(6) . ?
C5 C6 1.377(8) . ?
C5 H5 0.9300 . ?
C6 C38 1.462(9) . ?
C7 N1 1.502(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N1 1.502(7) . ?
C8 C9 1.504(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C14 1.370(8) . ?
C9 C10 1.421(8) . ?
C10 O2 1.312(7) . ?
C10 C11 1.415(8) . ?
C11 C12 1.402(9) . ?
C11 C15 1.462(9) . ?
C12 C13 1.354(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.407(9) . ?
C13 Cl2 1.740(7) . ?
C14 H14 0.9300 . ?
C15 N2 1.256(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.474(12) . ?
C16 N2 1.477(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.499(12) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 N3 1.473(9) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N3 1.281(9) . ?
C19 C20 1.446(11) . ?
C19 H19 0.9300 . ?
C20 C25 1.405(10) . ?
C20 C21 1.420(9) . ?
C21 O3 1.293(7) . ?
C21 C22 1.421(9) . ?
C22 C23 1.393(10) . ?
C22 C26 1.501(10) . ?
C23 C24 1.387(12) . ?
C23 H23 0.9300 . ?
C24 C25 1.346(12) . ?
C24 Cl3 1.745(8) . ?
C25 H25 0.9300 . ?
C26 N4 1.518(8) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.473(10) . ?
C27 N4 1.519(8) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.392(9) . ?
C28 C33 1.406(9) . ?
C29 O4 1.312(7) . ?
C29 C30 1.421(10) . ?
C30 C31 1.396(9) . ?
C30 C34 1.428(10) . ?
C31 C32 1.357(12) . ?
C31 H31 0.9300 . ?
C32 C33 1.357(12) . ?
C32 Cl4 1.755(7) . ?
C33 H33 0.9300 . ?
C34 N5 1.292(9) . ?
C34 H34 0.9300 . ?
C35 N5 1.456(9) . ?
C35 C36 1.509(12) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.540(11) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 N6 1.481(8) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 N6 1.270(8) . ?
C38 H38 0.9300 . ?
C39 C40 1.456(10) . ?
C39 N1 1.536(8) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.556(10) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C46 1.308(11) . ?
C41 C42 1.415(12) . ?
C42 C43 1.458(13) . ?
C42 H42 0.9300 . ?
C43 C44 1.360(14) . ?
C43 H43 0.9300 . ?
C44 C45 1.384(14) . ?
C44 H44 0.9300 . ?
C45 C46 1.281(12) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C47 C48 1.496(9) . ?
C47 N4 1.524(7) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 C49 1.533(9) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 C54 1.368(11) . ?
C49 C50 1.372(11) . ?
C50 C51 1.416(14) . ?
C50 H50 0.9300 . ?
C51 C52 1.338(16) . ?
C51 H51 0.9300 . ?
C52 C53 1.354(17) . ?
C52 H52 0.9300 . ?
C53 C54 1.384(14) . ?
C53 H53 0.9300 . ?
C54 H54 0.9300 . ?
N7 O6 1.220(7) . ?
N7 O7 1.229(7) . ?
N7 O5 1.329(6) . ?
N8 O9 1.210(10) . ?
N8 O8 1.212(11) . ?
N8 O10 1.265(13) . ?
O2 H2A 0.9700 . ?
O4 H4A 0.9701 . ?
O11 C55 1.29(3) . ?
O11 H11A 0.8500 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O4 91.18(16) . . ?
O1 Zn1 N5 143.11(19) . . ?
O4 Zn1 N5 90.5(2) . . ?
O1 Zn1 N6 86.71(18) . . ?
O4 Zn1 N6 174.0(2) . . ?
N5 Zn1 N6 87.8(2) . . ?
O1 Zn1 O5 101.60(16) . . ?
O4 Zn1 O5 92.12(17) . . ?
N5 Zn1 O5 115.16(19) . . ?
N6 Zn1 O5 93.81(19) . . ?
O2 Zn2 O3 95.50(16) . . ?
O2 Zn2 N3 120.91(19) . . ?
O3 Zn2 N3 91.5(2) . . ?
O2 Zn2 N2 90.11(18) . . ?
O3 Zn2 N2 173.43(18) . . ?
N3 Zn2 N2 88.6(2) . . ?
O2 Zn2 O5 113.85(16) . . ?
O3 Zn2 O5 87.98(16) . . ?
N3 Zn2 O5 125.01(19) . . ?
N2 Zn2 O5 86.62(19) . . ?
O1 C1 C6 124.2(5) . . ?
O1 C1 C2 118.2(5) . . ?
C6 C1 C2 117.5(5) . . ?
C3 C2 C1 121.7(5) . . ?
C3 C2 C7 121.3(5) . . ?
C1 C2 C7 116.9(5) . . ?
C2 C3 C4 118.4(6) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 121.1(6) . . ?
C5 C4 Cl1 121.0(5) . . ?
C3 C4 Cl1 117.8(5) . . ?
C4 C5 C6 121.4(6) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 119.7(6) . . ?
C5 C6 C38 118.1(6) . . ?
C1 C6 C38 122.1(5) . . ?
C2 C7 N1 111.1(5) . . ?
C2 C7 H7A 109.4 . . ?
N1 C7 H7A 109.4 . . ?
C2 C7 H7B 109.4 . . ?
N1 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N1 C8 C9 113.9(4) . . ?
N1 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
N1 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C14 C9 C10 121.2(6) . . ?
C14 C9 C8 121.1(5) . . ?
C10 C9 C8 117.7(5) . . ?
O2 C10 C11 124.4(5) . . ?
O2 C10 C9 117.6(5) . . ?
C11 C10 C9 118.0(6) . . ?
C12 C11 C10 119.4(6) . . ?
C12 C11 C15 116.8(6) . . ?
C10 C11 C15 123.7(6) . . ?
C13 C12 C11 121.2(6) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 120.7(6) . . ?
C12 C13 Cl2 120.7(6) . . ?
C14 C13 Cl2 118.6(5) . . ?
C9 C14 C13 119.5(6) . . ?
C9 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
N2 C15 C11 126.4(6) . . ?
N2 C15 H15 116.8 . . ?
C11 C15 H15 116.8 . . ?
C17 C16 N2 112.6(7) . . ?
C17 C16 H16A 109.1 . . ?
N2 C16 H16A 109.1 . . ?
C17 C16 H16B 109.1 . . ?
N2 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C16 C17 C18 118.9(7) . . ?
C16 C17 H17A 107.6 . . ?
C18 C17 H17A 107.6 . . ?
C16 C17 H17B 107.6 . . ?
C18 C17 H17B 107.6 . . ?
H17A C17 H17B 107.0 . . ?
N3 C18 C17 111.6(6) . . ?
N3 C18 H18A 109.3 . . ?
C17 C18 H18A 109.3 . . ?
N3 C18 H18B 109.3 . . ?
C17 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
N3 C19 C20 127.1(7) . . ?
N3 C19 H19 116.4 . . ?
C20 C19 H19 116.4 . . ?
C25 C20 C21 119.6(7) . . ?
C25 C20 C19 116.1(7) . . ?
C21 C20 C19 124.1(7) . . ?
O3 C21 C20 125.6(6) . . ?
O3 C21 C22 117.5(6) . . ?
C20 C21 C22 116.9(6) . . ?
C23 C22 C21 121.6(7) . . ?
C23 C22 C26 120.1(7) . . ?
C21 C22 C26 118.2(6) . . ?
C24 C23 C22 119.4(8) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C25 C24 C23 120.6(8) . . ?
C25 C24 Cl3 120.0(8) . . ?
C23 C24 Cl3 119.3(8) . . ?
C24 C25 C20 121.9(8) . . ?
C24 C25 H25 119.1 . . ?
C20 C25 H25 119.1 . . ?
C22 C26 N4 111.6(5) . . ?
C22 C26 H26A 109.3 . . ?
N4 C26 H26A 109.3 . . ?
C22 C26 H26B 109.3 . . ?
N4 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 N4 110.4(5) . . ?
C28 C27 H27A 109.6 . . ?
N4 C27 H27A 109.6 . . ?
C28 C27 H27B 109.6 . . ?
N4 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
C29 C28 C33 120.1(7) . . ?
C29 C28 C27 118.0(6) . . ?
C33 C28 C27 121.9(7) . . ?
O4 C29 C28 118.0(6) . . ?
O4 C29 C30 123.7(6) . . ?
C28 C29 C30 118.2(6) . . ?
C31 C30 C29 119.8(8) . . ?
C31 C30 C34 115.6(7) . . ?
C29 C30 C34 124.5(6) . . ?
C32 C31 C30 120.2(8) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C33 C32 C31 121.5(7) . . ?
C33 C32 Cl4 119.3(8) . . ?
C31 C32 Cl4 119.1(7) . . ?
C32 C33 C28 120.2(8) . . ?
C32 C33 H33 119.9 . . ?
C28 C33 H33 119.9 . . ?
N5 C34 C30 127.5(6) . . ?
N5 C34 H34 116.3 . . ?
C30 C34 H34 116.3 . . ?
N5 C35 C36 110.4(6) . . ?
N5 C35 H35A 109.6 . . ?
C36 C35 H35A 109.6 . . ?
N5 C35 H35B 109.6 . . ?
C36 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
C35 C36 C37 112.6(6) . . ?
C35 C36 H36A 109.1 . . ?
C37 C36 H36A 109.1 . . ?
C35 C36 H36B 109.1 . . ?
C37 C36 H36B 109.1 . . ?
H36A C36 H36B 107.8 . . ?
N6 C37 C36 111.7(6) . . ?
N6 C37 H37A 109.3 . . ?
C36 C37 H37A 109.3 . . ?
N6 C37 H37B 109.3 . . ?
C36 C37 H37B 109.3 . . ?
H37A C37 H37B 107.9 . . ?
N6 C38 C6 126.5(6) . . ?
N6 C38 H38 116.7 . . ?
C6 C38 H38 116.7 . . ?
C40 C39 N1 114.6(6) . . ?
C40 C39 H39A 108.6 . . ?
N1 C39 H39A 108.6 . . ?
C40 C39 H39B 108.6 . . ?
N1 C39 H39B 108.6 . . ?
H39A C39 H39B 107.6 . . ?
C39 C40 C41 114.0(7) . . ?
C39 C40 H40A 108.8 . . ?
C41 C40 H40A 108.8 . . ?
C39 C40 H40B 108.8 . . ?
C41 C40 H40B 108.8 . . ?
H40A C40 H40B 107.6 . . ?
C46 C41 C42 120.2(8) . . ?
C46 C41 C40 121.7(8) . . ?
C42 C41 C40 118.0(8) . . ?
C41 C42 C43 117.6(9) . . ?
C41 C42 H42 121.2 . . ?
C43 C42 H42 121.2 . . ?
C44 C43 C42 117.1(10) . . ?
C44 C43 H43 121.4 . . ?
C42 C43 H43 121.4 . . ?
C43 C44 C45 119.8(9) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C46 C45 C44 122.7(11) . . ?
C46 C45 H45 118.7 . . ?
C44 C45 H45 118.7 . . ?
C45 C46 C41 122.6(11) . . ?
C45 C46 H46 118.7 . . ?
C41 C46 H46 118.7 . . ?
C48 C47 N4 112.2(5) . . ?
C48 C47 H47A 109.2 . . ?
N4 C47 H47A 109.2 . . ?
C48 C47 H47B 109.2 . . ?
N4 C47 H47B 109.2 . . ?
H47A C47 H47B 107.9 . . ?
C47 C48 C49 110.1(5) . . ?
C47 C48 H48A 109.6 . . ?
C49 C48 H48A 109.6 . . ?
C47 C48 H48B 109.6 . . ?
C49 C48 H48B 109.6 . . ?
H48A C48 H48B 108.2 . . ?
C54 C49 C50 118.7(8) . . ?
C54 C49 C48 120.1(8) . . ?
C50 C49 C48 121.2(7) . . ?
C49 C50 C51 120.1(10) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
C52 C51 C50 119.0(11) . . ?
C52 C51 H51 120.5 . . ?
C50 C51 H51 120.5 . . ?
C51 C52 C53 121.8(11) . . ?
C51 C52 H52 119.1 . . ?
C53 C52 H52 119.1 . . ?
C52 C53 C54 119.4(11) . . ?
C52 C53 H53 120.3 . . ?
C54 C53 H53 120.3 . . ?
C49 C54 C53 121.0(10) . . ?
C49 C54 H54 119.5 . . ?
C53 C54 H54 119.5 . . ?
C8 N1 C7 113.0(5) . . ?
C8 N1 C39 110.1(5) . . ?
C7 N1 C39 107.9(5) . . ?
C15 N2 C16 119.0(6) . . ?
C15 N2 Zn2 125.3(4) . . ?
C16 N2 Zn2 115.7(5) . . ?
C19 N3 C18 119.0(6) . . ?
C19 N3 Zn2 124.5(5) . . ?
C18 N3 Zn2 116.3(5) . . ?
C26 N4 C27 109.8(5) . . ?
C26 N4 C47 113.7(5) . . ?
C27 N4 C47 112.8(5) . . ?
C34 N5 C35 117.8(6) . . ?
C34 N5 Zn1 124.3(5) . . ?
C35 N5 Zn1 117.7(5) . . ?
C38 N6 C37 116.3(6) . . ?
C38 N6 Zn1 122.6(4) . . ?
C37 N6 Zn1 119.7(4) . . ?
O6 N7 O7 122.3(6) . . ?
O6 N7 O5 119.1(5) . . ?
O7 N7 O5 118.6(5) . . ?
O9 N8 O8 122.2(12) . . ?
O9 N8 O10 120.1(10) . . ?
O8 N8 O10 117.7(10) . . ?
C1 O1 Zn1 126.7(3) . . ?
C10 O2 Zn2 128.6(4) . . ?
C10 O2 H2A 104.8 . . ?
Zn2 O2 H2A 104.9 . . ?
C21 O3 Zn2 126.9(4) . . ?
C29 O4 Zn1 129.3(4) . . ?
C29 O4 H4A 104.5 . . ?
Zn1 O4 H4A 104.7 . . ?
N7 O5 Zn1 116.5(3) . . ?
N7 O5 Zn2 110.7(3) . . ?
Zn1 O5 Zn2 124.50(19) . . ?
C55 O11 H11A 98.2 . . ?
O11 C55 H55A 110.8 . . ?
O11 C55 H55B 106.0 . . ?
H55A C55 H55B 109.5 . . ?
O11 C55 H55C 111.6 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         3.265
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.101
_database_code_depnum_ccdc_archive 'CCDC 955029'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H25 Cl2 N3 O3 Pb'
_chemical_formula_sum            'C27 H25 Cl2 N3 O3 Pb'
_chemical_formula_weight         717.59

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.404(3)
_cell_length_b                   10.422(3)
_cell_length_c                   13.660(4)
_cell_angle_alpha                98.637(5)
_cell_angle_beta                 102.317(5)
_cell_angle_gamma                99.253(4)
_cell_volume                     1401.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    2859
_cell_measurement_theta_min      2.248
_cell_measurement_theta_max      23.249

_exptl_crystal_description       block
_exptl_crystal_colour            'orange yellow'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    6.240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5742
_exptl_absorpt_correction_T_max  0.6352
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'

_exptl_special_details           
; 
The structure was solved by direct methods (Bruker, 2000) and
successive difference Fourier syntheses.
;

_diffrn_ambient_temperature      291(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 CCD area detector'
_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            7799
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4919
_reflns_number_gt                3715
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (BRUKER 2000)'
_computing_cell_refinement       'SMART APEX2 V2011.4-1'
_computing_data_reduction        'SAINT V6.02A (BRUKER 2000)'
_computing_structure_solution    'SHELXTL V6.10 (BRUKER 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0379P)²] 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         4919
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0836
_refine_ls_wR_factor_gt          0.0802
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.916
_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
Pb1 Pb 1.02570(3) 0.28684(3) 0.73229(2) 0.05705(11) Uani 1 1 d . . .
C1 C 1.0057(6) 0.5726(6) 0.8620(4) 0.0402(14) Uani 1 1 d . . .
C2 C 1.0337(6) 0.7087(6) 0.8561(4) 0.0434(14) Uani 1 1 d . B .
C3 C 0.9588(6) 0.7935(7) 0.8913(5) 0.0530(17) Uani 1 1 d . . .
H3 H 0.9773 0.8822 0.8861 0.064 Uiso 1 1 calc R . .
C4 C 0.8556(6) 0.7483(7) 0.9347(5) 0.0552(17) Uani 1 1 d . . .
C5 C 0.8227(6) 0.6189(7) 0.9389(5) 0.0506(16) Uani 1 1 d . . .
H5 H 0.7521 0.5900 0.9671 0.061 Uiso 1 1 calc R . .
C6 C 0.8944(6) 0.5273(6) 0.9009(4) 0.0433(15) Uani 1 1 d . . .
C7 C 0.8464(6) 0.3882(7) 0.9025(5) 0.0519(16) Uani 1 1 d . . .
H7 H 0.7837 0.3708 0.9406 0.062 Uiso 1 1 calc R . .
C8 C 0.8096(8) 0.1562(7) 0.8615(5) 0.065(2) Uani 1 1 d . . .
H8AA H 0.7791 0.1591 0.9232 0.078 Uiso 0.50 1 d PR A 1
H8AB H 0.8701 0.0958 0.8599 0.078 Uiso 0.50 1 d PR A 1
H8BC H 0.7241 0.1619 0.8759 0.078 Uiso 0.50 1 d PR A 2
H8BD H 0.8628 0.1225 0.9146 0.078 Uiso 0.50 1 d PR A 2
C9 C 0.6934(15) 0.1106(14) 0.7721(12) 0.058(4) Uani 0.50 1 d P B 1
H9A H 0.6320 0.1709 0.7770 0.070 Uiso 0.50 1 calc PR B 1
H9B H 0.6472 0.0245 0.7779 0.070 Uiso 0.50 1 calc PR B 1
C9' C 0.774(2) 0.0626(18) 0.7618(13) 0.089(6) Uani 0.50 1 d P B 2
H9'A H 0.8556 0.0325 0.7538 0.107 Uiso 0.50 1 calc PR B 2
H9'B H 0.7123 -0.0140 0.7684 0.107 Uiso 0.50 1 calc PR B 2
C10 C 0.7177(8) 0.0988(7) 0.6684(6) 0.074(2) Uani 1 1 d . . .
H10A H 0.7747 0.0359 0.6611 0.088 Uiso 0.50 1 d PR B 1
H10B H 0.6337 0.0682 0.6185 0.088 Uiso 0.50 1 d PR B 1
H10C H 0.7126 0.0317 0.6105 0.088 Uiso 0.50 1 d PR B 2
H10D H 0.6287 0.1045 0.6751 0.088 Uiso 0.50 1 d PR B 2
C11 C 0.7091(7) 0.3077(6) 0.6223(5) 0.0544(17) Uani 1 1 d . . .
H11 H 0.6168 0.2763 0.6047 0.065 Uiso 1 1 calc R B .
C12 C 0.7562(6) 0.4428(6) 0.6127(4) 0.0445(15) Uani 1 1 d . B .
C13 C 0.6629(6) 0.5248(7) 0.6042(5) 0.0526(17) Uani 1 1 d . . .
H13 H 0.5733 0.4893 0.5993 0.063 Uiso 1 1 calc R B .
C14 C 0.7001(6) 0.6566(6) 0.6030(4) 0.0467(15) Uani 1 1 d . B .
C15 C 0.8307(6) 0.7120(6) 0.6111(4) 0.0470(15) Uani 1 1 d . . .
H15 H 0.8551 0.8019 0.6113 0.056 Uiso 1 1 calc R B .
C16 C 0.9270(6) 0.6339(7) 0.6190(4) 0.0462(15) Uani 1 1 d . B .
C17 C 0.8914(6) 0.4975(6) 0.6169(4) 0.0445(15) Uani 1 1 d . . .
C18 C 1.0709(6) 0.6917(7) 0.6250(5) 0.0564(18) Uani 1 1 d . . .
H18A H 1.0796 0.7850 0.6222 0.068 Uiso 1 1 calc R B .
H18B H 1.0967 0.6483 0.5663 0.068 Uiso 1 1 calc R . .
C19 C 1.1524(6) 0.7593(7) 0.8169(5) 0.0599(18) Uani 1 1 d . . .
H19A H 1.1472 0.8477 0.8043 0.072 Uiso 1 1 calc R B .
H19B H 1.2333 0.7667 0.8699 0.072 Uiso 1 1 calc R . .
C20 C 1.3069(6) 0.7059(8) 0.7082(5) 0.0609(19) Uani 1 1 d . . .
H20A H 1.3359 0.8010 0.7169 0.073 Uiso 1 1 calc R B .
H20B H 1.3070 0.6670 0.6391 0.073 Uiso 1 1 calc R . .
C21 C 1.4070(7) 0.6536(9) 0.7827(6) 0.076(2) Uani 1 1 d . B .
H21A H 1.4965 0.6861 0.7754 0.091 Uiso 1 1 calc R . .
H21B H 1.4037 0.6899 0.8516 0.091 Uiso 1 1 calc R . .
C22 C 1.3851(6) 0.5070(9) 0.7701(5) 0.061(2) Uani 1 1 d . . .
C23 C 1.4242(8) 0.4514(11) 0.8552(6) 0.089(3) Uani 1 1 d . B .
H23 H 1.4568 0.5078 0.9184 0.106 Uiso 1 1 calc R . .
C24 C 1.4179(10) 0.3239(13) 0.8518(9) 0.102(3) Uani 1 1 d . . .
H24 H 1.4431 0.2933 0.9122 0.122 Uiso 1 1 calc R B .
C25 C 1.3753(9) 0.2354(12) 0.7616(11) 0.103(3) Uani 1 1 d . B .
C26 C 1.3318(9) 0.2846(11) 0.6703(8) 0.094(3) Uani 1 1 d . . .
H26 H 1.3011 0.2276 0.6072 0.113 Uiso 1 1 calc R B .
C27 C 1.3366(7) 0.4198(9) 0.6784(6) 0.075(2) Uani 1 1 d . B .
H27 H 1.3061 0.4524 0.6198 0.090 Uiso 1 1 calc R . .
Cl1 Cl 0.7684(2) 0.8617(2) 0.9851(2) 0.0941(7) Uani 1 1 d . . .
Cl2 Cl 0.57850(16) 0.75616(17) 0.59169(14) 0.0630(5) Uani 1 1 d . . .
N1 N 1.1654(4) 0.6764(5) 0.7216(4) 0.0470(13) Uani 1 1 d . B .
N2 N 0.8806(5) 0.2900(5) 0.8582(4) 0.0531(13) Uani 1 1 d . B .
N3 N 0.7831(5) 0.2278(5) 0.6527(4) 0.0561(14) Uani 1 1 d . B .
O1 O 0.9855(4) 0.4270(4) 0.6210(3) 0.0568(11) Uani 1 1 d . B .
O2 O 1.0854(4) 0.4967(4) 0.8350(3) 0.0537(11) Uani 1 1 d . . .
O3 O 1.3691(8) 0.1026(8) 0.7513(8) 0.150(3) Uani 1 1 d . . .
H3A H 1.3114 0.0657 0.6961 0.225 Uiso 1 1 d R B .


_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
#C9 H8BC 1.3875 . ? 
#C9 H10D 1.3385 . ? 
#C9' H8AB 1.4452 . ? 
#C9' H10A 1.3629 . ? 
Pb1 O1 2.283(4) . ?
Pb1 O2 2.325(4) . ?
Pb1 N3 2.461(5) . ?
Pb1 N2 2.519(5) . ?
C1 O2 1.305(7) . ?
C1 C6 1.418(8) . ?
C1 C2 1.419(8) . ?
C2 C3 1.369(9) . ?
C2 C19 1.499(8) . ?
C3 C4 1.384(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.351(9) . ?
C4 Cl1 1.750(7) . ?
C5 C6 1.407(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.460(9) . ?
C7 N2 1.250(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.481(16) . ?
C8 N2 1.481(8) . ?
C8 C9' 1.488(19) . ?
C8 H8AA 0.9601 . ?
C8 H8AB 0.9599 . ?
C8 H8BC 0.9600 . ?
C8 H8BD 0.9601 . ?
C9 C10 1.481(18) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9' C10 1.418(18) . ?
C9' H9'A 0.9700 . ?
C9' H9'B 0.9700 . ?
C10 N3 1.473(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9601 . ?
C10 H10C 0.9600 . ?
C10 H10D 0.9601 . ?
C11 N3 1.277(8) . ?
C11 C12 1.450(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.390(9) . ?
C12 C17 1.416(8) . ?
C13 C14 1.369(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.362(8) . ?
C14 Cl2 1.757(6) . ?
C15 C16 1.386(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.405(9) . ?
C16 C18 1.501(8) . ?
C17 O1 1.313(7) . ?
C18 N1 1.514(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N1 1.495(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N1 1.511(7) . ?
C20 C21 1.522(9) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.486(11) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C27 1.375(11) . ?
C22 C23 1.389(10) . ?
C23 C24 1.313(13) . ?
C23 H23 0.9300 . ?
C24 C25 1.364(15) . ?
C24 H24 0.9300 . ?
C25 O3 1.360(12) . ?
C25 C26 1.431(14) . ?
C26 C27 1.388(12) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
O3 H3A 0.8499 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
#C9 C8 C9' 42.2(9) . . ? 
#C8 C9 H8BC 38.9 . . ? 
#C10 C9 H10D 39.4 . . ? 
#C8 C9' H8AB 38.2 . . ? 
#C10 C9' H10A 40.3 . . ? 
#C9' C10 C9 43.2(9) . . ? 
O1 Pb1 O2 75.59(15) . . ?
O1 Pb1 N3 74.07(17) . . ?
O2 Pb1 N3 111.57(16) . . ?
O1 Pb1 N2 113.41(16) . . ?
O2 Pb1 N2 72.85(16) . . ?
N3 Pb1 N2 65.98(17) . . ?
O2 C1 C6 123.3(6) . . ?
O2 C1 C2 119.0(5) . . ?
C6 C1 C2 117.7(5) . . ?
C3 C2 C1 120.6(5) . . ?
C3 C2 C19 120.7(6) . . ?
C1 C2 C19 118.6(6) . . ?
C2 C3 C4 120.5(6) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 120.8(6) . . ?
C5 C4 Cl1 120.1(5) . . ?
C3 C4 Cl1 119.0(6) . . ?
C4 C5 C6 120.6(6) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 119.5(6) . . ?
C5 C6 C7 116.9(6) . . ?
C1 C6 C7 123.6(6) . . ?
N2 C7 C6 127.0(6) . . ?
N2 C7 H7 116.5 . . ?
C6 C7 H7 116.5 . . ?
C9 C8 N2 109.7(7) . . ?
N2 C8 C9' 113.6(9) . . ?
C9 C8 H8AA 109.6 . . ?
N2 C8 H8AA 109.5 . . ?
C9' C8 H8AA 134.7 . . ?
C9 C8 H8AB 109.2 . . ?
N2 C8 H8AB 109.3 . . ?
C9' C8 H8AB 68.5 . . ?
H8AA C8 H8AB 109.5 . . ?
C9 C8 H8BC 65.3 . . ?
N2 C8 H8BC 109.3 . . ?
C9' C8 H8BC 103.6 . . ?
H8AA C8 H8BC 47.5 . . ?
H8AB C8 H8BC 140.3 . . ?
C9 C8 H8BD 140.4 . . ?
N2 C8 H8BD 108.9 . . ?
C9' C8 H8BD 111.8 . . ?
H8AA C8 H8BD 64.7 . . ?
H8AB C8 H8BD 48.0 . . ?
H8BC C8 H8BD 109.5 . . ?
C8 C9 C10 118.7(11) . . ?
C10 C9 H8BC 154.1 . . ?
C8 C9 H9A 107.6 . . ?
C10 C9 H9A 107.6 . . ?
H8BC C9 H9A 77.1 . . ?
C8 C9 H9B 107.6 . . ?
C10 C9 H9B 107.6 . . ?
H8BC C9 H9B 94.6 . . ?
H9A C9 H9B 107.1 . . ?
C8 C9 H10D 153.6 . . ?
H8BC C9 H10D 152.9 . . ?
H9A C9 H10D 75.9 . . ?
H9B C9 H10D 95.7 . . ?
C10 C9' C8 122.5(15) . . ?
C10 C9' H8AB 149.3 . . ?
C10 C9' H9'A 106.7 . . ?
C8 C9' H9'A 106.7 . . ?
H8AB C9' H9'A 71.6 . . ?
C10 C9' H9'B 106.7 . . ?
C8 C9' H9'B 106.7 . . ?
H8AB C9' H9'B 102.9 . . ?
H9'A C9' H9'B 106.6 . . ?
C8 C9' H10A 150.4 . . ?
H8AB C9' H10A 138.4 . . ?
H9'A C9' H10A 69.7 . . ?
H9'B C9' H10A 102.4 . . ?
C9' C10 N3 115.3(9) . . ?
N3 C10 C9 110.6(8) . . ?
C9' C10 H10A 66.7 . . ?
N3 C10 H10A 109.5 . . ?
C9 C10 H10A 108.6 . . ?
C9' C10 H10B 133.7 . . ?
N3 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 109.5 . . ?
C9' C10 H10C 112.0 . . ?
N3 C10 H10C 109.4 . . ?
C9 C10 H10C 139.6 . . ?
H10A C10 H10C 51.2 . . ?
H10B C10 H10C 61.3 . . ?
C9' C10 H10D 101.8 . . ?
N3 C10 H10D 108.5 . . ?
C9 C10 H10D 62.2 . . ?
H10A C10 H10D 141.6 . . ?
H10B C10 H10D 50.8 . . ?
H10C C10 H10D 109.5 . . ?
N3 C11 C12 125.9(6) . . ?
N3 C11 H11 117.1 . . ?
C12 C11 H11 117.1 . . ?
C13 C12 C17 118.5(6) . . ?
C13 C12 C11 117.2(6) . . ?
C17 C12 C11 124.1(6) . . ?
C14 C13 C12 121.4(6) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C15 C14 C13 120.8(6) . . ?
C15 C14 Cl2 119.4(5) . . ?
C13 C14 Cl2 119.8(5) . . ?
C14 C15 C16 119.8(6) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C17 120.8(5) . . ?
C15 C16 C18 120.9(6) . . ?
C17 C16 C18 118.3(6) . . ?
O1 C17 C16 118.5(5) . . ?
O1 C17 C12 123.0(6) . . ?
C16 C17 C12 118.5(6) . . ?
C16 C18 N1 112.5(5) . . ?
C16 C18 H18A 109.1 . . ?
N1 C18 H18A 109.1 . . ?
C16 C18 H18B 109.1 . . ?
N1 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
N1 C19 C2 115.4(5) . . ?
N1 C19 H19A 108.4 . . ?
C2 C19 H19A 108.4 . . ?
N1 C19 H19B 108.4 . . ?
C2 C19 H19B 108.4 . . ?
H19A C19 H19B 107.5 . . ?
N1 C20 C21 113.4(5) . . ?
N1 C20 H20A 108.9 . . ?
C21 C20 H20A 108.9 . . ?
N1 C20 H20B 108.9 . . ?
C21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C22 C21 C20 115.2(6) . . ?
C22 C21 H21A 108.5 . . ?
C20 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
C20 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
C27 C22 C23 116.0(9) . . ?
C27 C22 C21 125.1(7) . . ?
C23 C22 C21 118.8(8) . . ?
C24 C23 C22 124.0(10) . . ?
C24 C23 H23 118.0 . . ?
C22 C23 H23 118.0 . . ?
C23 C24 C25 121.4(10) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.3 . . ?
O3 C25 C24 125.0(12) . . ?
O3 C25 C26 116.9(12) . . ?
C24 C25 C26 118.1(10) . . ?
C27 C26 C25 118.2(10) . . ?
C27 C26 H26 120.9 . . ?
C25 C26 H26 120.9 . . ?
C22 C27 C26 122.3(8) . . ?
C22 C27 H27 118.9 . . ?
C26 C27 H27 118.9 . . ?
C19 N1 C20 111.3(5) . . ?
C19 N1 C18 114.3(5) . . ?
C20 N1 C18 107.9(4) . . ?
C7 N2 C8 118.3(6) . . ?
C7 N2 Pb1 127.6(5) . . ?
C8 N2 Pb1 113.0(4) . . ?
C11 N3 C10 118.4(6) . . ?
C11 N3 Pb1 125.8(4) . . ?
C10 N3 Pb1 113.7(4) . . ?
C17 O1 Pb1 124.7(4) . . ?
C1 O2 Pb1 127.7(4) . . ?
C25 O3 H3A 107.4 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.998
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.104
_database_code_depnum_ccdc_archive 'CCDC 955030'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H26 Cl2 N3 O2 Pb, N O3'
_chemical_formula_sum            'C27 H26 Cl2 N4 O5 Pb'
_chemical_formula_weight         764.61

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'

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

_cell_length_a                   20.254(8)
_cell_length_b                   10.682(3)
_cell_length_c                   13.612(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.762(8)
_cell_angle_gamma                90.00
_cell_volume                     2910.6(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    3893
_cell_measurement_theta_min      2.548
_cell_measurement_theta_max      24.825

_exptl_crystal_description       block
_exptl_crystal_colour            'orange yellow'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488
_exptl_absorpt_coefficient_mu    6.023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5842
_exptl_absorpt_correction_T_max  0.5842
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'

_exptl_special_details           
; 
The structure was solved by direct methods (Bruker, 2000) and
successive difference Fourier syntheses.
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7752
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2696
_reflns_number_gt                2349
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (BRUKER 2000)'
_computing_cell_refinement       'SMART APEX2 V2011.4-1'
_computing_data_reduction        'SAINT V6.02A (BRUKER 2000)'
_computing_structure_solution    'SHELXTL V6.10 (BRUKER 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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. In this structure, the 
 largest Q1 peak is very close to the Pb(II) center with the Pb-Q separation 
 of only 0.798 Ang. So we think a large residual peak of 4.486 may 
 be acceptable. In addition, two restrains are used to fix the bond lengths
 of alkyl chain of pendant arm in the macrocyclic ligand, namely, 
 'DFIX 1.52 0.01 C12 C11' and 'DFIX 1.50 0.01 C12 C13'.
;

_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)+(0.0498P)²+94.6839P] 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         2696
_refine_ls_number_parameters     194
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.1659
_refine_ls_wR_factor_gt          0.1626
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.082
_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
Pb1 Pb 0.11686(4) 0.0000 0.60010(5) 0.0447(3) Uani 1 2 d S . .
C1 C 0.2564(6) 0.1539(9) 0.6730(8) 0.036(2) Uani 1 1 d . . .
C2 C 0.2449(6) 0.1852(10) 0.7718(8) 0.035(2) Uani 1 1 d . . .
C3 C 0.2979(6) 0.2189(11) 0.8434(9) 0.045(3) Uani 1 1 d . . .
H3 H 0.2900 0.2436 0.9061 0.053 Uiso 1 1 calc R . .
C4 C 0.3608(6) 0.2162(13) 0.8227(8) 0.049(3) Uani 1 1 d . . .
C5 C 0.3745(6) 0.1794(11) 0.7290(9) 0.046(3) Uani 1 1 d . . .
H5 H 0.4184 0.1767 0.7163 0.055 Uiso 1 1 calc R . .
C6 C 0.3231(6) 0.1477(10) 0.6567(8) 0.037(3) Uani 1 1 d . . .
C7 C 0.1785(6) 0.1829(11) 0.8014(9) 0.045(3) Uani 1 1 d . . .
H7 H 0.1735 0.2248 0.8597 0.054 Uiso 1 1 calc R . .
C8 C 0.0668(7) 0.1212(14) 0.8071(11) 0.061(4) Uani 1 1 d . . .
H8A H 0.0266 0.1251 0.7583 0.074 Uiso 1 1 calc R . .
H8B H 0.0666 0.1922 0.8514 0.074 Uiso 1 1 calc R . .
C9 C 0.0669(11) 0.0000 0.8667(17) 0.069(6) Uani 1 2 d S . .
H9A H 0.1059 0.0000 0.9177 0.083 Uiso 1 2 calc SR . .
H9B H 0.0278 0.0000 0.9000 0.083 Uiso 1 2 calc SR . .
C10 C 0.3368(6) 0.1193(11) 0.5532(9) 0.045(3) Uani 1 1 d . . .
H10A H 0.3846 0.1114 0.5545 0.054 Uiso 1 1 calc R . .
H10B H 0.3213 0.1888 0.5098 0.054 Uiso 1 1 calc R . .
C11 C 0.2977(8) 0.0000 0.3985(13) 0.058(5) Uani 1 2 d SD . .
H11A H 0.2735 0.0736 0.3711 0.070 Uiso 0.50 1 calc PR . .
H11B H 0.2735 -0.0736 0.3711 0.070 Uiso 0.50 1 calc PR . .
C12 C 0.3680(8) 0.0000 0.3715(12) 0.058(6) Uani 1 2 d SD . .
H12A H 0.3924 -0.0738 0.3979 0.069 Uiso 0.50 1 calc PR . .
H12B H 0.3924 0.0738 0.3979 0.069 Uiso 0.50 1 calc PR . .
C13 C 0.3586(12) 0.0000 0.2575(12) 0.064(6) Uani 1 2 d SD . .
C14 C 0.2975(12) 0.0000 0.1848(15) 0.060(5) Uani 1 2 d S . .
H14 H 0.2570 0.0000 0.2091 0.072 Uiso 1 2 calc SR . .
C15 C 0.2952(16) 0.0000 0.0804(17) 0.078(7) Uani 1 2 d S . .
H15 H 0.2547 0.0000 0.0377 0.093 Uiso 1 2 calc SR . .
C16 C 0.355(2) 0.0000 0.0445(18) 0.099(11) Uani 1 2 d S . .
H16 H 0.3556 0.0000 -0.0237 0.119 Uiso 1 2 calc SR . .
C17 C 0.4123(19) 0.0000 0.107(2) 0.098(10) Uani 1 2 d S . .
H17 H 0.4523 0.0000 0.0814 0.117 Uiso 1 2 calc SR . .
C18 C 0.4141(14) 0.0000 0.2092(17) 0.076(7) Uani 1 2 d S . .
H18 H 0.4558 0.0000 0.2486 0.091 Uiso 1 2 calc SR . .
Cl1 Cl 0.4277(2) 0.2580(5) 0.9158(3) 0.0837(14) Uani 1 1 d . . .
N1 N 0.1267(5) 0.1291(10) 0.7551(7) 0.045(2) Uani 1 1 d . . .
N2 N 0.3029(7) 0.0000 0.5114(9) 0.040(3) Uani 1 2 d S . .
N3 N 0.0000 0.235(2) 0.5000 0.20(3) Uani 1 2 d S . .
O1 O 0.2082(4) 0.1325(7) 0.5996(6) 0.0411(18) Uani 1 1 d . . .
H1A H 0.2274 0.1074 0.5519 0.062 Uiso 0.50 1 d PR . .
O2 O 0.0266(14) 0.192(3) 0.445(2) 0.212(12) Uani 1 1 d . . .
O3 O 0.0000 0.346(6) 0.5000 0.29(3) 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
Pb1 O1 2.331(8) . ?
Pb1 O1 2.331(8) 6 ?
Pb1 N1 2.503(10) . ?
Pb1 N1 2.503(10) 6 ?
Pb1 O2 3.29(3) . ?
C1 O1 1.306(14) . ?
C1 C6 1.404(16) . ?
C1 C2 1.439(14) . ?
C2 C3 1.383(17) . ?
C2 C7 1.461(16) . ?
C3 C4 1.347(17) . ?
C3 H3 0.9300 . ?
C4 C5 1.402(17) . ?
C4 Cl1 1.765(12) . ?
C5 C6 1.363(17) . ?
C5 H5 0.9300 . ?
C6 C10 1.507(15) . ?
C7 N1 1.275(16) . ?
C7 H7 0.9300 . ?
C8 N1 1.497(15) . ?
C8 C9 1.528(18) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C8 1.528(18) 6 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.518(14) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.52(2) . ?
C11 C12 1.524(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.534(10) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C18 1.39(3) . ?
C13 C14 1.46(3) . ?
C14 C15 1.42(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.38(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.33(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.39(3) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
N2 C10 1.518(14) 6 ?
N3 O2 1.09(3) . ?
N3 O2 1.09(3) 2_556 ?
N3 O3 1.18(6) . ?
O1 H1A 0.8500 . ?

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
O1 Pb1 O1 74.8(4) . 6 ?
O1 Pb1 N1 72.9(3) . . ?
O1 Pb1 N1 112.1(3) 6 . ?
O1 Pb1 N1 112.1(3) . 6 ?
O1 Pb1 N1 72.9(3) 6 6 ?
N1 Pb1 N1 66.9(5) . 6 ?
O1 Pb1 O2 89.0(5) . . ?
O1 Pb1 O2 137.7(5) 6 . ?
N1 Pb1 O2 99.4(6) . . ?
N1 Pb1 O2 148.2(5) 6 . ?
O1 C1 C6 119.7(9) . . ?
O1 C1 C2 123.2(10) . . ?
C6 C1 C2 117.1(10) . . ?
C3 C2 C1 120.0(10) . . ?
C3 C2 C7 117.3(10) . . ?
C1 C2 C7 122.7(11) . . ?
C4 C3 C2 120.3(11) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 121.4(11) . . ?
C3 C4 Cl1 119.4(9) . . ?
C5 C4 Cl1 119.1(10) . . ?
C6 C5 C4 119.4(11) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 121.5(10) . . ?
C5 C6 C10 119.7(11) . . ?
C1 C6 C10 118.4(10) . . ?
N1 C7 C2 126.4(11) . . ?
N1 C7 H7 116.8 . . ?
C2 C7 H7 116.8 . . ?
N1 C8 C9 111.3(12) . . ?
N1 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C8 C9 C8 115.8(18) 6 . ?
C8 C9 H9A 108.3 6 . ?
C8 C9 H9A 108.3 . . ?
C8 C9 H9B 108.3 6 . ?
C8 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C6 C10 N2 112.5(9) . . ?
C6 C10 H10A 109.1 . . ?
N2 C10 H10A 109.1 . . ?
C6 C10 H10B 109.1 . . ?
N2 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N2 C11 C12 108.6(13) . . ?
N2 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
N2 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.3 . . ?
C11 C12 C13 105.5(15) . . ?
C11 C12 H12A 110.6 . . ?
C13 C12 H12A 110.6 . . ?
C11 C12 H12B 110.6 . . ?
C13 C12 H12B 110.6 . . ?
H12A C12 H12B 108.8 . . ?
C18 C13 C14 110.0(17) . . ?
C18 C13 C12 120(2) . . ?
C14 C13 C12 130.3(18) . . ?
C15 C14 C13 125(2) . . ?
C15 C14 H14 117.4 . . ?
C13 C14 H14 117.4 . . ?
C16 C15 C14 117(3) . . ?
C16 C15 H15 121.3 . . ?
C14 C15 H15 121.3 . . ?
C17 C16 C15 120(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 122(3) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
C13 C18 C17 125(3) . . ?
C13 C18 H18 117.4 . . ?
C17 C18 H18 117.4 . . ?
C7 N1 C8 117.2(11) . . ?
C7 N1 Pb1 128.3(8) . . ?
C8 N1 Pb1 113.6(8) . . ?
C10 N2 C10 114.3(14) . 6 ?
C10 N2 C11 109.7(7) . . ?
C10 N2 C11 109.7(7) 6 . ?
O2 N3 O2 130(4) . 2_556 ?
O2 N3 O3 115.1(19) . . ?
O2 N3 O3 115.1(19) 2_556 . ?
C1 O1 Pb1 127.2(6) . . ?
C1 O1 H1A 105.3 . . ?
Pb1 O1 H1A 105.4 . . ?
N3 O2 Pb1 96.2(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -173.4(10) . . . . ?
C6 C1 C2 C3 6.0(15) . . . . ?
O1 C1 C2 C7 6.7(16) . . . . ?
C6 C1 C2 C7 -173.9(10) . . . . ?
C1 C2 C3 C4 -3.6(18) . . . . ?
C7 C2 C3 C4 176.3(11) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C2 C3 C4 Cl1 -179.3(10) . . . . ?
C3 C4 C5 C6 1(2) . . . . ?
Cl1 C4 C5 C6 -179.7(10) . . . . ?
C4 C5 C6 C1 1.6(18) . . . . ?
C4 C5 C6 C10 174.5(11) . . . . ?
O1 C1 C6 C5 174.4(10) . . . . ?
C2 C1 C6 C5 -5.0(16) . . . . ?
O1 C1 C6 C10 1.4(15) . . . . ?
C2 C1 C6 C10 -178.0(9) . . . . ?
C3 C2 C7 N1 -163.3(12) . . . . ?
C1 C2 C7 N1 16.5(19) . . . . ?
N1 C8 C9 C8 -59(2) . . . 6 ?
C5 C6 C10 N2 132.6(12) . . . . ?
C1 C6 C10 N2 -54.2(15) . . . . ?
N2 C11 C12 C13 180.000(2) . . . . ?
C11 C12 C13 C18 180.000(2) . . . . ?
C11 C12 C13 C14 0.000(2) . . . . ?
C18 C13 C14 C15 0.000(2) . . . . ?
C12 C13 C14 C15 180.000(2) . . . . ?
C13 C14 C15 C16 0.000(1) . . . . ?
C14 C15 C16 C17 0.000(2) . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
C14 C13 C18 C17 0.000(2) . . . . ?
C12 C13 C18 C17 180.000(2) . . . . ?
C16 C17 C18 C13 0.000(2) . . . . ?
C2 C7 N1 C8 170.4(12) . . . . ?
C2 C7 N1 Pb1 2.4(18) . . . . ?
C9 C8 N1 C7 -91.4(16) . . . . ?
C9 C8 N1 Pb1 78.4(15) . . . . ?
O1 Pb1 N1 C7 -24.3(10) . . . . ?
O1 Pb1 N1 C7 40.8(11) 6 . . . ?
N1 Pb1 N1 C7 99.6(10) 6 . . . ?
O2 Pb1 N1 C7 -110.4(11) . . . . ?
O1 Pb1 N1 C8 167.3(9) . . . . ?
O1 Pb1 N1 C8 -127.6(8) 6 . . . ?
N1 Pb1 N1 C8 -68.8(9) 6 . . . ?
O2 Pb1 N1 C8 81.3(9) . . . . ?
C6 C10 N2 C10 -76.1(15) . . . 6 ?
C6 C10 N2 C11 160.3(11) . . . . ?
C12 C11 N2 C10 63.1(9) . . . . ?
C12 C11 N2 C10 -63.1(9) . . . 6 ?
C6 C1 O1 Pb1 131.2(9) . . . . ?
C2 C1 O1 Pb1 -49.4(13) . . . . ?
O1 Pb1 O1 C1 -72.2(9) 6 . . . ?
N1 Pb1 O1 C1 47.1(8) . . . . ?
N1 Pb1 O1 C1 -8.2(9) 6 . . . ?
O2 Pb1 O1 C1 147.3(10) . . . . ?
O2 N3 O2 Pb1 -50.1(5) 2_556 . . . ?
O3 N3 O2 Pb1 129.9(5) . . . . ?
O1 Pb1 O2 N3 -103(2) . . . . ?
O1 Pb1 O2 N3 -168.8(15) 6 . . . ?
N1 Pb1 O2 N3 -30(2) . . . . ?
N1 Pb1 O2 N3 30(3) 6 . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         4.486
_refine_diff_density_min         -3.031
_refine_diff_density_rms         0.211
_database_code_depnum_ccdc_archive 'CCDC 955031'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H58 Cl4 N2 O12 Zn2'
_chemical_formula_sum            'C54 H58 Cl4 N2 O12 Zn2'
_chemical_formula_weight         1199.60

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   'P 21/c '
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.255(7)
_cell_length_b                   15.508(9)
_cell_length_c                   17.377(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.50(3)
_cell_angle_gamma                90.00
_cell_volume                     2802(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    1355
_cell_measurement_theta_min      2.627
_cell_measurement_theta_max      27.812

_exptl_crystal_description       block
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8973
_exptl_absorpt_correction_T_max  0.8973
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'

_exptl_special_details           
; 
The structure was solved by direct methods (Bruker, 2000) and
successive difference Fourier syntheses.
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15461
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.2088
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4843
_reflns_number_gt                1811
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (BRUKER 2000)'
_computing_cell_refinement       'SMART APEX2 V2011.4-1'
_computing_data_reduction        'SAINT V6.02A (BRUKER 2000)'
_computing_structure_solution    'SHELXTL V6.10 (BRUKER 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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. Six carbon atoms of the 
 phenyl ring in the pendant arm have relatively large Ueq, so six restraints 
 are used here: DELU 0.001 C21 C26; DELU 0.001 C21 C22; DELU 0.001 C22 C23;  
 DELU 0.001 C25 C26; DELU 0.001 C23 C24; DELU 0.001 C25 C24.
;

_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)+(0.0606P)²] 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         4843
_refine_ls_number_parameters     337
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.2268
_refine_ls_R_factor_gt           0.0761
_refine_ls_wR_factor_ref         0.1776
_refine_ls_wR_factor_gt          0.1358
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_restrained_S_all      0.879
_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
Zn1 Zn -0.06921(8) 0.44653(6) 0.54989(5) 0.0544(3) Uani 1 1 d . . .
C1 C -0.2329(6) 0.5544(5) 0.3915(4) 0.0507(19) Uani 1 1 d . . .
C2 C -0.3514(7) 0.5159(6) 0.3914(5) 0.063(2) Uani 1 1 d . . .
C3 C -0.4734(7) 0.5452(6) 0.3309(5) 0.074(3) Uani 1 1 d . . .
H3 H -0.5493 0.5213 0.3307 0.089 Uiso 1 1 calc R . .
C4 C -0.4787(7) 0.6070(6) 0.2746(5) 0.066(2) Uani 1 1 d . . .
C5 C -0.3645(7) 0.6465(5) 0.2762(5) 0.065(2) Uani 1 1 d . . .
H5 H -0.3696 0.6899 0.2381 0.078 Uiso 1 1 calc R . .
C6 C -0.2431(7) 0.6213(5) 0.3343(4) 0.055(2) Uani 1 1 d . . .
C7 C -0.3550(8) 0.4508(6) 0.4503(5) 0.076(3) Uani 1 1 d . . .
H7 H -0.4374 0.4333 0.4437 0.091 Uiso 1 1 calc R . .
C8 C -0.1257(7) 0.6757(5) 0.3375(4) 0.059(2) Uani 1 1 d . . .
H8A H -0.1536 0.7145 0.2901 0.070 Uiso 1 1 calc R . .
H8B H -0.0984 0.7109 0.3874 0.070 Uiso 1 1 calc R . .
C9 C -0.0559(7) 0.5618(5) 0.2660(4) 0.059(2) Uani 1 1 d . . .
H9A H -0.0990 0.5933 0.2145 0.071 Uiso 1 1 calc R . .
H9B H -0.1189 0.5241 0.2740 0.071 Uiso 1 1 calc R . .
C10 C 0.0511(7) 0.5053(5) 0.2560(5) 0.053(2) Uani 1 1 d . . .
C11 C 0.1159(7) 0.4465(6) 0.3229(5) 0.057(2) Uani 1 1 d . . .
C12 C 0.2111(7) 0.3908(5) 0.3126(5) 0.058(2) Uani 1 1 d . . .
C13 C 0.2340(7) 0.3931(5) 0.2396(6) 0.062(2) Uani 1 1 d . . .
H13 H 0.2944 0.3560 0.2330 0.074 Uiso 1 1 calc R . .
C14 C 0.1675(8) 0.4502(6) 0.1765(5) 0.064(2) Uani 1 1 d . . .
C15 C 0.0756(8) 0.5058(6) 0.1844(5) 0.063(2) Uani 1 1 d . . .
H15 H 0.0308 0.5432 0.1412 0.076 Uiso 1 1 calc R . .
C16 C 0.2829(8) 0.3289(6) 0.3827(6) 0.077(3) Uani 1 1 d . . .
H16 H 0.3028 0.3577 0.4364 0.092 Uiso 1 1 calc R . .
C17 C 0.2046(11) 0.2162(8) 0.4538(7) 0.139(5) Uani 1 1 d . . .
H17A H 0.2583 0.1659 0.4660 0.208 Uiso 1 1 calc R . .
H17B H 0.1189 0.2000 0.4472 0.208 Uiso 1 1 calc R . .
H17C H 0.2382 0.2567 0.4988 0.208 Uiso 1 1 calc R . .
C18 C 0.4883(10) 0.2522(8) 0.4486(7) 0.145(5) Uani 1 1 d . . .
H18A H 0.5006 0.2827 0.4992 0.217 Uiso 1 1 calc R . .
H18B H 0.5695 0.2461 0.4429 0.217 Uiso 1 1 calc R . .
H18C H 0.4531 0.1962 0.4503 0.217 Uiso 1 1 calc R . .
C19 C 0.0806(7) 0.6884(5) 0.3218(4) 0.062(2) Uani 1 1 d . . .
H19A H 0.0373 0.7140 0.2672 0.074 Uiso 1 1 calc R . .
H19B H 0.1540 0.6565 0.3205 0.074 Uiso 1 1 calc R . .
C20 C 0.1301(8) 0.7610(6) 0.3856(5) 0.074(3) Uani 1 1 d . . .
H20A H 0.1640 0.7356 0.4407 0.089 Uiso 1 1 calc R . .
H20B H 0.0577 0.7969 0.3821 0.089 Uiso 1 1 calc R . .
C21 C 0.2347(8) 0.8195(6) 0.3766(5) 0.075(2) Uani 1 1 d U . .
C22 C 0.2507(10) 0.8994(6) 0.4102(8) 0.129(5) Uani 1 1 d U . .
H22 H 0.1967 0.9183 0.4360 0.155 Uiso 1 1 calc R . .
C23 C 0.3483(13) 0.9547(9) 0.4066(11) 0.170(7) Uani 1 1 d U . .
H23 H 0.3579 1.0092 0.4306 0.204 Uiso 1 1 calc R . .
C24 C 0.4298(15) 0.9296(12) 0.3681(9) 0.168(7) Uani 1 1 d U . .
H24 H 0.4989 0.9632 0.3694 0.202 Uiso 1 1 calc R . .
C25 C 0.4040(14) 0.8573(13) 0.3309(8) 0.196(10) Uani 1 1 d U . .
H25 H 0.4486 0.8424 0.2975 0.235 Uiso 1 1 calc R . .
C26 C 0.3128(11) 0.7983(9) 0.3365(7) 0.135(5) Uani 1 1 d U . .
H26 H 0.3059 0.7441 0.3124 0.162 Uiso 1 1 calc R . .
C27 C -0.1427(9) 0.3014(7) 0.3922(5) 0.116(4) Uani 1 1 d . . .
H27A H -0.2147 0.2884 0.4069 0.174 Uiso 1 1 calc R . .
H27B H -0.1105 0.2491 0.3778 0.174 Uiso 1 1 calc R . .
H27C H -0.1695 0.3399 0.3454 0.174 Uiso 1 1 calc R . .
Cl1 Cl -0.6275(2) 0.6381(2) 0.19703(17) 0.1136(10) Uani 1 1 d . . .
Cl3 Cl 0.1893(3) 0.4487(2) 0.08011(15) 0.1104(10) Uani 1 1 d . . .
N1 N -0.0099(5) 0.6258(4) 0.3371(3) 0.0507(16) Uani 1 1 d . . .
O1 O -0.1179(4) 0.5246(3) 0.4426(3) 0.0544(14) Uani 1 1 d . . .
O2 O -0.2665(5) 0.4138(4) 0.5086(3) 0.0761(18) Uani 1 1 d . . .
O3 O -0.0417(5) 0.3421(3) 0.4626(3) 0.0677(16) Uani 1 1 d . . .
H3A H 0.0151 0.3686 0.4392 0.102 Uiso 1 1 d R . .
O4 O 0.0931(4) 0.4430(3) 0.3935(3) 0.0608(14) Uani 1 1 d . . .
O5 O 0.2021(7) 0.2557(5) 0.3773(4) 0.105(2) Uani 1 1 d . . .
O6 O 0.3979(6) 0.3015(4) 0.3761(3) 0.091(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
Zn1 O4 2.044(5) 3_566 ?
Zn1 O1 2.107(5) 3_566 ?
Zn1 O1 2.112(5) . ?
Zn1 O2 2.117(5) . ?
Zn1 N1 2.137(6) 3_566 ?
Zn1 O3 2.319(5) . ?
Zn1 Zn1 3.202(2) 3_566 ?
C1 O1 1.341(8) . ?
C1 C6 1.411(10) . ?
C1 C2 1.460(10) . ?
C2 C3 1.447(10) . ?
C2 C7 1.450(11) . ?
C3 C4 1.355(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.415(10) . ?
C4 Cl1 1.768(8) . ?
C5 C6 1.408(9) . ?
C5 H5 0.9300 . ?
C6 C8 1.550(10) . ?
C7 O2 1.254(9) . ?
C7 H7 0.9300 . ?
C8 N1 1.517(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N1 1.514(8) . ?
C9 C10 1.552(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C15 1.373(9) . ?
C10 C11 1.437(10) . ?
C11 O4 1.348(8) . ?
C11 C12 1.439(10) . ?
C12 C13 1.389(10) . ?
C12 C16 1.519(11) . ?
C13 C14 1.385(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.393(11) . ?
C14 Cl3 1.784(7) . ?
C15 H15 0.9300 . ?
C16 O6 1.408(9) . ?
C16 O5 1.435(10) . ?
C16 H16 0.9800 . ?
C17 O5 1.454(10) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 O6 1.492(10) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N1 1.504(9) . ?
C19 C20 1.528(10) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.540(11) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.352(12) . ?
C21 C26 1.355(13) . ?
C22 C23 1.414(16) . ?
C22 H22 0.9300 . ?
C23 C24 1.38(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.27(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.406(15) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 O3 1.458(8) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
N1 Zn1 2.137(6) 3_566 ?
O1 Zn1 2.107(5) 3_566 ?
O3 H3A 0.9700 . ?
O4 Zn1 2.044(5) 3_566 ?

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
O4 Zn1 O1 95.97(19) 3_566 3_566 ?
O4 Zn1 O1 84.7(2) 3_566 . ?
O1 Zn1 O1 81.29(18) 3_566 . ?
O4 Zn1 O2 92.9(2) 3_566 . ?
O1 Zn1 O2 164.87(19) 3_566 . ?
O1 Zn1 O2 87.4(2) . . ?
O4 Zn1 N1 94.8(2) 3_566 3_566 ?
O1 Zn1 N1 89.95(19) 3_566 3_566 ?
O1 Zn1 N1 171.10(19) . 3_566 ?
O2 Zn1 N1 101.5(2) . 3_566 ?
O4 Zn1 O3 167.19(19) 3_566 . ?
O1 Zn1 O3 78.96(18) 3_566 . ?
O1 Zn1 O3 82.93(19) . . ?
O2 Zn1 O3 89.8(2) . . ?
N1 Zn1 O3 97.0(2) 3_566 . ?
O4 Zn1 Zn1 90.42(15) 3_566 3_566 ?
O1 Zn1 Zn1 40.70(12) 3_566 3_566 ?
O1 Zn1 Zn1 40.59(13) . 3_566 ?
O2 Zn1 Zn1 127.23(16) . 3_566 ?
N1 Zn1 Zn1 130.63(16) 3_566 3_566 ?
O3 Zn1 Zn1 78.04(13) . 3_566 ?
O1 C1 C6 121.2(6) . . ?
O1 C1 C2 120.7(7) . . ?
C6 C1 C2 118.1(7) . . ?
C3 C2 C7 117.2(8) . . ?
C3 C2 C1 119.0(8) . . ?
C7 C2 C1 123.8(7) . . ?
C4 C3 C2 121.0(8) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 120.2(7) . . ?
C3 C4 Cl1 120.7(7) . . ?
C5 C4 Cl1 119.1(7) . . ?
C6 C5 C4 121.2(8) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C1 120.3(7) . . ?
C5 C6 C8 117.0(8) . . ?
C1 C6 C8 122.4(6) . . ?
O2 C7 C2 131.3(8) . . ?
O2 C7 H7 114.4 . . ?
C2 C7 H7 114.4 . . ?
N1 C8 C6 116.4(7) . . ?
N1 C8 H8A 108.2 . . ?
C6 C8 H8A 108.2 . . ?
N1 C8 H8B 108.2 . . ?
C6 C8 H8B 108.2 . . ?
H8A C8 H8B 107.3 . . ?
N1 C9 C10 115.1(6) . . ?
N1 C9 H9A 108.5 . . ?
C10 C9 H9A 108.5 . . ?
N1 C9 H9B 108.5 . . ?
C10 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C15 C10 C11 121.4(8) . . ?
C15 C10 C9 122.1(7) . . ?
C11 C10 C9 116.3(7) . . ?
O4 C11 C10 123.2(8) . . ?
O4 C11 C12 119.9(8) . . ?
C10 C11 C12 116.9(7) . . ?
C13 C12 C11 120.3(8) . . ?
C13 C12 C16 121.4(8) . . ?
C11 C12 C16 118.3(8) . . ?
C14 C13 C12 120.4(8) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 121.0(7) . . ?
C13 C14 Cl3 120.5(7) . . ?
C15 C14 Cl3 118.3(7) . . ?
C10 C15 C14 120.0(8) . . ?
C10 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
O6 C16 O5 109.6(8) . . ?
O6 C16 C12 110.4(7) . . ?
O5 C16 C12 108.6(7) . . ?
O6 C16 H16 109.4 . . ?
O5 C16 H16 109.4 . . ?
C12 C16 H16 109.4 . . ?
O5 C17 H17A 109.5 . . ?
O5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 C20 115.5(6) . . ?
N1 C19 H19A 108.4 . . ?
C20 C19 H19A 108.4 . . ?
N1 C19 H19B 108.4 . . ?
C20 C19 H19B 108.4 . . ?
H19A C19 H19B 107.5 . . ?
C19 C20 C21 116.2(7) . . ?
C19 C20 H20A 108.2 . . ?
C21 C20 H20A 108.2 . . ?
C19 C20 H20B 108.2 . . ?
C21 C20 H20B 108.2 . . ?
H20A C20 H20B 107.4 . . ?
C22 C21 C26 116.0(10) . . ?
C22 C21 C20 118.5(10) . . ?
C26 C21 C20 125.5(10) . . ?
C21 C22 C23 121.0(13) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C24 C23 C22 121.4(15) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C25 C24 C23 115.5(15) . . ?
C25 C24 H24 122.2 . . ?
C23 C24 H24 122.2 . . ?
C24 C25 C26 124.7(16) . . ?
C24 C25 H25 117.7 . . ?
C26 C25 H25 117.7 . . ?
C21 C26 C25 120.8(13) . . ?
C21 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
O3 C27 H27A 109.5 . . ?
O3 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O3 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C19 N1 C9 108.7(5) . . ?
C19 N1 C8 108.3(6) . . ?
C9 N1 C8 108.2(5) . . ?
C19 N1 Zn1 115.4(4) . 3_566 ?
C9 N1 Zn1 107.4(4) . 3_566 ?
C8 N1 Zn1 108.7(4) . 3_566 ?
C1 O1 Zn1 131.0(5) . 3_566 ?
C1 O1 Zn1 129.8(5) . . ?
Zn1 O1 Zn1 98.71(18) 3_566 . ?
C7 O2 Zn1 124.8(6) . . ?
C27 O3 Zn1 126.5(5) . . ?
C27 O3 H3A 104.9 . . ?
Zn1 O3 H3A 104.7 . . ?
C11 O4 Zn1 120.7(5) . 3_566 ?
C16 O5 C17 118.8(8) . . ?
C16 O6 C18 116.0(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -175.1(7) . . . . ?
C6 C1 C2 C3 2.5(11) . . . . ?
O1 C1 C2 C7 6.5(12) . . . . ?
C6 C1 C2 C7 -175.9(7) . . . . ?
C7 C2 C3 C4 178.8(8) . . . . ?
C1 C2 C3 C4 0.4(12) . . . . ?
C2 C3 C4 C5 -2.4(13) . . . . ?
C2 C3 C4 Cl1 176.3(6) . . . . ?
C3 C4 C5 C6 1.7(13) . . . . ?
Cl1 C4 C5 C6 -177.1(6) . . . . ?
C4 C5 C6 C1 1.3(11) . . . . ?
C4 C5 C6 C8 -173.1(7) . . . . ?
O1 C1 C6 C5 174.3(7) . . . . ?
C2 C1 C6 C5 -3.3(11) . . . . ?
O1 C1 C6 C8 -11.6(11) . . . . ?
C2 C1 C6 C8 170.8(7) . . . . ?
C3 C2 C7 O2 180.0(9) . . . . ?
C1 C2 C7 O2 -1.7(15) . . . . ?
C5 C6 C8 N1 -132.1(7) . . . . ?
C1 C6 C8 N1 53.6(9) . . . . ?
N1 C9 C10 C15 -120.3(8) . . . . ?
N1 C9 C10 C11 65.1(9) . . . . ?
C15 C10 C11 O4 -178.8(7) . . . . ?
C9 C10 C11 O4 -4.2(11) . . . . ?
C15 C10 C11 C12 2.5(11) . . . . ?
C9 C10 C11 C12 177.1(7) . . . . ?
O4 C11 C12 C13 179.1(7) . . . . ?
C10 C11 C12 C13 -2.2(11) . . . . ?
O4 C11 C12 C16 0.3(11) . . . . ?
C10 C11 C12 C16 179.0(7) . . . . ?
C11 C12 C13 C14 1.4(12) . . . . ?
C16 C12 C13 C14 -179.9(7) . . . . ?
C12 C13 C14 C15 -0.7(12) . . . . ?
C12 C13 C14 Cl3 -176.0(6) . . . . ?
C11 C10 C15 C14 -1.9(13) . . . . ?
C9 C10 C15 C14 -176.2(7) . . . . ?
C13 C14 C15 C10 1.0(13) . . . . ?
Cl3 C14 C15 C10 176.4(6) . . . . ?
C13 C12 C16 O6 21.0(11) . . . . ?
C11 C12 C16 O6 -160.2(7) . . . . ?
C13 C12 C16 O5 -99.1(9) . . . . ?
C11 C12 C16 O5 79.6(9) . . . . ?
N1 C19 C20 C21 173.2(7) . . . . ?
C19 C20 C21 C22 157.7(9) . . . . ?
C19 C20 C21 C26 -21.5(14) . . . . ?
C26 C21 C22 C23 -3.2(18) . . . . ?
C20 C21 C22 C23 177.6(11) . . . . ?
C21 C22 C23 C24 1(2) . . . . ?
C22 C23 C24 C25 6(3) . . . . ?
C23 C24 C25 C26 -9(3) . . . . ?
C22 C21 C26 C25 -0.2(18) . . . . ?
C20 C21 C26 C25 179.0(12) . . . . ?
C24 C25 C26 C21 7(3) . . . . ?
C20 C19 N1 C9 176.5(6) . . . . ?
C20 C19 N1 C8 59.2(8) . . . . ?
C20 C19 N1 Zn1 -62.8(8) . . . 3_566 ?
C10 C9 N1 C19 62.3(8) . . . . ?
C10 C9 N1 C8 179.6(6) . . . . ?
C10 C9 N1 Zn1 -63.2(7) . . . 3_566 ?
C6 C8 N1 C19 167.9(6) . . . . ?
C6 C8 N1 C9 50.3(8) . . . . ?
C6 C8 N1 Zn1 -66.0(6) . . . 3_566 ?
C6 C1 O1 Zn1 -5.6(10) . . . 3_566 ?
C2 C1 O1 Zn1 172.0(5) . . . 3_566 ?
C6 C1 O1 Zn1 165.3(5) . . . . ?
C2 C1 O1 Zn1 -17.1(10) . . . . ?
O4 Zn1 O1 C1 -76.2(6) 3_566 . . . ?
O1 Zn1 O1 C1 -173.1(7) 3_566 . . . ?
O2 Zn1 O1 C1 17.0(6) . . . . ?
N1 Zn1 O1 C1 -163.1(12) 3_566 . . . ?
O3 Zn1 O1 C1 107.1(6) . . . . ?
Zn1 Zn1 O1 C1 -173.1(7) 3_566 . . . ?
O4 Zn1 O1 Zn1 96.9(2) 3_566 . . 3_566 ?
O1 Zn1 O1 Zn1 0.0 3_566 . . 3_566 ?
O2 Zn1 O1 Zn1 -170.0(2) . . . 3_566 ?
N1 Zn1 O1 Zn1 10.0(14) 3_566 . . 3_566 ?
O3 Zn1 O1 Zn1 -79.9(2) . . . 3_566 ?
C2 C7 O2 Zn1 6.9(13) . . . . ?
O4 Zn1 O2 C7 73.5(7) 3_566 . . . ?
O1 Zn1 O2 C7 -52.3(12) 3_566 . . . ?
O1 Zn1 O2 C7 -11.0(7) . . . . ?
N1 Zn1 O2 C7 169.0(7) 3_566 . . . ?
O3 Zn1 O2 C7 -93.9(7) . . . . ?
Zn1 Zn1 O2 C7 -19.2(8) 3_566 . . . ?
O4 Zn1 O3 C27 -84.6(10) 3_566 . . . ?
O1 Zn1 O3 C27 -152.3(6) 3_566 . . . ?
O1 Zn1 O3 C27 -69.8(6) . . . . ?
O2 Zn1 O3 C27 17.6(6) . . . . ?
N1 Zn1 O3 C27 119.2(6) 3_566 . . . ?
Zn1 Zn1 O3 C27 -110.7(6) 3_566 . . . ?
C10 C11 O4 Zn1 -41.2(9) . . . 3_566 ?
C12 C11 O4 Zn1 137.5(6) . . . 3_566 ?
O6 C16 O5 C17 96.2(9) . . . . ?
C12 C16 O5 C17 -143.1(8) . . . . ?
O5 C16 O6 C18 -70.3(10) . . . . ?
C12 C16 O6 C18 170.2(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.094



#===END
_database_code_depnum_ccdc_archive 'CCDC 1009728'
