# Electronic Supplementary Material (ESI) for Polymer Chemistry
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               Polym.Chem.

_journal_coden_Cambridge         1478

_publ_contact_author_name        'McKeown, Neil B.'
_publ_contact_author_email       mckeownnb@cardiff.ac.uk

_publ_section_title              
;
Enhancing the rigidity of a network polymer of intrinsic microporosity
by the combined use of phthalocyanine and triptycene components.
;
loop_
_publ_author_name
N.B.McKeown
M.Hashem
C.Bezzu
B.Kariuki

# Attachment '- 831067_PC.txt'

data_nbm1035
_database_code_depnum_ccdc_archive 'CCDC 831067'
#TrackingRef '- 831067_PC.txt'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C132.31 H129.21 Cl32.03 N8 O17.63 Zn'
_chemical_formula_weight         3314.28

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.0853(6)
_cell_length_b                   18.0594(6)
_cell_length_c                   18.6508(9)
_cell_angle_alpha                79.027(3)
_cell_angle_beta                 75.275(2)
_cell_angle_gamma                72.973(3)
_cell_volume                     4043.7(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1695
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22912
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_sigmaI/netI    0.1026
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.14
_diffrn_reflns_theta_max         25.94
_reflns_number_total             15100
_reflns_number_gt                9528
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.041(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         15100
_refine_ls_number_parameters     629
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.2130
_refine_ls_R_factor_gt           0.1629
_refine_ls_wR_factor_ref         0.4765
_refine_ls_wR_factor_gt          0.4436
_refine_ls_goodness_of_fit_ref   1.651
_refine_ls_restrained_S_all      1.653
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0392(6) 1.0235(4) 0.3440(4) 0.0427(18) Uiso 1 1 d . A 1
C2 C -0.1025(6) 1.0797(4) 0.2931(4) 0.0416(17) Uiso 1 1 d . A 1
C3 C -0.1659(6) 1.1404(4) 0.3356(4) 0.0431(18) Uiso 1 1 d . . 1
C4 C 0.1374(6) 0.8777(4) 0.5928(4) 0.0418(17) Uiso 1 1 d . . 1
C5 C -0.1052(6) 1.0798(5) 0.2201(4) 0.0442(18) Uiso 1 1 d . A 1
H5 H -0.0618 1.0392 0.1931 0.053 Uiso 1 1 calc R A 1
C6 C -0.1762(6) 1.1438(4) 0.1884(4) 0.0412(17) Uiso 1 1 d . A 1
C7 C -0.2411(6) 1.2062(4) 0.2308(4) 0.0415(17) Uiso 1 1 d . A 1
C8 C -0.2366(6) 1.2048(4) 0.3029(4) 0.0398(17) Uiso 1 1 d . A 1
H8 H -0.2794 1.2455 0.3300 0.048 Uiso 1 1 calc R A 1
C9 C -0.1868(6) 1.1571(4) 0.1057(4) 0.0418(17) Uiso 0.322(5) 1 d P A 1
C10 C -0.3098(6) 1.2735(4) 0.1834(4) 0.0407(17) Uiso 1 1 d . A 1
C11 C -0.1604(6) 1.2362(4) 0.0759(4) 0.0410(17) Uiso 1 1 d . A 1
C12 C -0.2234(6) 1.2979(5) 0.1168(4) 0.0460(19) Uiso 1 1 d . A 1
C13 C -0.1997(6) 1.3681(4) 0.1011(4) 0.0388(17) Uiso 1 1 d . A 1
H13 H -0.2388 1.4075 0.1306 0.047 Uiso 1 1 calc R A 1
C14 C -0.1163(7) 1.3811(5) 0.0402(4) 0.0460(19) Uiso 1 1 d . A 1
C15 C -0.0544(6) 1.3220(5) -0.0018(4) 0.0447(18) Uiso 1 1 d . A 1
C16 C -0.0747(6) 1.2495(5) 0.0162(4) 0.0442(18) Uiso 1 1 d . A 1
H16 H -0.0315 1.2091 -0.0111 0.053 Uiso 1 1 calc R A 1
C17 C -0.3742(6) 1.2333(4) 0.1512(4) 0.0438(18) Uiso 1 1 d . A 1
C18 C -0.3096(6) 1.1739(4) 0.1101(4) 0.0412(17) Uiso 1 1 d . A 1
C19 C -0.3592(6) 1.1352(4) 0.0755(4) 0.0405(17) Uiso 1 1 d . A 1
H19 H -0.3162 1.0960 0.0467 0.049 Uiso 1 1 calc R A 1
C20 C -0.4717(7) 1.1551(5) 0.0843(4) 0.0455(18) Uiso 1 1 d . A 1
C21 C -0.5364(7) 1.2122(5) 0.1287(5) 0.050(2) Uiso 1 1 d . A 1
C22 C -0.4882(6) 1.2513(4) 0.1633(4) 0.0427(18) Uiso 1 1 d . A 1
H22 H -0.5314 1.2889 0.1939 0.051 Uiso 1 1 calc R A 1
C23 C -0.1141(7) 1.0899(5) 0.0611(4) 0.0450(18) Uiso 0.322(5) 1 d P A 1
H23A H -0.1369 1.0428 0.0842 0.054 Uiso 0.322(5) 1 calc PR A 1
H23B H -0.0395 1.0815 0.0662 0.054 Uiso 0.322(5) 1 calc PR A 1
C24 C -0.114(3) 1.1009(19) -0.0287(17) 0.067(3) Uiso 0.322(5) 1 d P A 1
H24A H -0.0659 1.0555 -0.0503 0.100 Uiso 0.322(5) 1 calc PR A 1
H24B H -0.0889 1.1462 -0.0531 0.100 Uiso 0.322(5) 1 calc PR A 1
H24C H -0.1866 1.1073 -0.0351 0.100 Uiso 0.322(5) 1 calc PR A 1
C25 C -0.3812(7) 1.3411(5) 0.2306(4) 0.0467(19) Uiso 1 1 d . A 1
H25A H -0.4288 1.3194 0.2730 0.056 Uiso 1 1 calc R A 1
H25B H -0.3328 1.3600 0.2501 0.056 Uiso 1 1 calc R A 1
C26 C -0.4515(8) 1.4105(5) 0.1897(5) 0.057(2) Uiso 1 1 d . A 1
H26A H -0.4663 1.3942 0.1481 0.086 Uiso 1 1 calc R A 1
H26B H -0.4134 1.4507 0.1720 0.086 Uiso 1 1 calc R A 1
H26C H -0.5192 1.4303 0.2233 0.086 Uiso 1 1 calc R A 1
C27 C -0.1499(7) 1.5146(5) 0.0620(5) 0.055(2) Uiso 1 1 d . A 1
H27A H -0.2256 1.5226 0.0617 0.082 Uiso 1 1 calc R A 1
H27B H -0.1274 1.5612 0.0393 0.082 Uiso 1 1 calc R A 1
H27C H -0.1399 1.5024 0.1125 0.082 Uiso 1 1 calc R A 1
C28 C 0.0868(7) 1.2842(5) -0.1087(5) 0.055(2) Uiso 1 1 d . A 1
H28A H 0.1255 1.2385 -0.0814 0.083 Uiso 1 1 calc R A 1
H28B H 0.1382 1.3059 -0.1472 0.083 Uiso 1 1 calc R A 1
H28C H 0.0374 1.2704 -0.1308 0.083 Uiso 1 1 calc R A 1
C29 C -0.7168(8) 1.2911(6) 0.1750(5) 0.061(2) Uiso 1 1 d . A 1
H29A H -0.7149 1.2789 0.2271 0.092 Uiso 1 1 calc R A 1
H29B H -0.7906 1.3007 0.1692 0.092 Uiso 1 1 calc R A 1
H29C H -0.6907 1.3368 0.1547 0.092 Uiso 1 1 calc R A 1
C30 C -0.4674(8) 1.0916(6) -0.0183(5) 0.066(2) Uiso 1 1 d . A 1
H30A H -0.4311 1.1286 -0.0503 0.099 Uiso 1 1 calc R A 1
H30B H -0.5181 1.0820 -0.0424 0.099 Uiso 1 1 calc R A 1
H30C H -0.4143 1.0436 -0.0081 0.099 Uiso 1 1 calc R A 1
C31 C 0.0834(6) 0.9031(4) 0.3731(4) 0.0434(18) Uiso 1 1 d . A 1
C32 C 0.1543(6) 0.8264(4) 0.3547(4) 0.0429(18) Uiso 1 1 d . A 1
C33 C 0.1974(6) 0.7882(4) 0.4165(4) 0.0415(17) Uiso 1 1 d . A 1
C34 C 0.1538(6) 0.8431(4) 0.4731(4) 0.0404(17) Uiso 1 1 d . A 1
C35 C 0.1822(7) 0.7899(5) 0.2904(5) 0.050(2) Uiso 1 1 d . A 1
H35 H 0.1542 0.8151 0.2484 0.060 Uiso 1 1 calc R A 1
C36 C 0.2522(6) 0.7156(5) 0.2898(4) 0.0444(18) Uiso 1 1 d . A 1
C37 C 0.2904(6) 0.6757(4) 0.3556(4) 0.0407(17) Uiso 1 1 d . A 1
C38 C 0.2635(6) 0.7132(4) 0.4193(4) 0.0425(18) Uiso 1 1 d . A 1
H38 H 0.2893 0.6885 0.4621 0.051 Uiso 1 1 calc R A 1
C39 C 0.2977(7) 0.6704(5) 0.2215(5) 0.0478(19) Uiso 0.678(5) 1 d P A 1
C40 C 0.3647(6) 0.5937(4) 0.3464(4) 0.0365(16) Uiso 1 1 d . A 1
C41 C 0.4248(6) 0.6485(4) 0.2157(4) 0.0418(17) Uiso 1 1 d . A 1
C42 C 0.4617(6) 0.6079(4) 0.2819(4) 0.0403(17) Uiso 1 1 d . A 1
C43 C 0.5660(6) 0.5880(4) 0.2845(4) 0.0423(18) Uiso 1 1 d . A 1
H43 H 0.5881 0.5607 0.3279 0.051 Uiso 1 1 calc R A 1
C44 C 0.6439(6) 0.6078(4) 0.2224(4) 0.0429(18) Uiso 1 1 d . A 1
C45 C 0.6107(7) 0.6491(5) 0.1593(5) 0.050(2) Uiso 1 1 d . A 1
C46 C 0.5028(6) 0.6687(4) 0.1546(4) 0.0392(17) Uiso 1 1 d . A 1
H46 H 0.4818 0.6954 0.1107 0.047 Uiso 1 1 calc R A 1
C47 C 0.2689(6) 0.5900(5) 0.2502(4) 0.0454(18) Uiso 1 1 d . A 1
C48 C 0.3038(6) 0.5506(4) 0.3158(4) 0.0397(17) Uiso 1 1 d . A 1
C49 C 0.2846(6) 0.4788(4) 0.3440(4) 0.0409(17) Uiso 1 1 d . A 1
H49 H 0.3101 0.4513 0.3862 0.049 Uiso 1 1 calc R A 1
C50 C 0.2267(6) 0.4465(4) 0.3094(4) 0.0427(18) Uiso 1 1 d . A 1
C51 C 0.1857(7) 0.4891(5) 0.2466(4) 0.0464(19) Uiso 1 1 d . A 1
C52 C 0.2093(6) 0.5591(4) 0.2167(4) 0.0417(17) Uiso 1 1 d . A 1
H52 H 0.1855 0.5862 0.1738 0.050 Uiso 1 1 calc R A 1
C53 C 0.2612(7) 0.7108(5) 0.1523(5) 0.051(2) Uiso 0.678(5) 1 d P A 1
H53A H 0.1853 0.7107 0.1587 0.061 Uiso 0.678(5) 1 calc PR A 1
H53B H 0.3030 0.6798 0.1123 0.061 Uiso 0.678(5) 1 calc PR A 1
C54 C 0.270(2) 0.7927(16) 0.1270(16) 0.137(9) Uiso 0.678(5) 1 d P A 1
H54A H 0.2425 0.8118 0.0819 0.206 Uiso 0.678(5) 1 calc PR A 1
H54B H 0.3447 0.7940 0.1177 0.206 Uiso 0.678(5) 1 calc PR A 1
H54C H 0.2270 0.8250 0.1650 0.206 Uiso 0.678(5) 1 calc PR A 1
C55 C 0.4040(6) 0.5494(4) 0.4180(4) 0.0388(17) Uiso 1 1 d . A 1
H55A H 0.4536 0.4995 0.4061 0.047 Uiso 1 1 calc R A 1
H55B H 0.4456 0.5788 0.4318 0.047 Uiso 1 1 calc R A 1
C56 C 0.3154(7) 0.5340(5) 0.4860(5) 0.052(2) Uiso 1 1 d . A 1
H56A H 0.2448 0.5558 0.4737 0.078 Uiso 1 1 calc R A 1
H56B H 0.3195 0.5578 0.5267 0.078 Uiso 1 1 calc R A 1
H56C H 0.3264 0.4787 0.5003 0.078 Uiso 1 1 calc R A 1
C57 C 0.7924(9) 0.5400(6) 0.2818(6) 0.067(3) Uiso 1 1 d . A 1
H57A H 0.7708 0.5671 0.3250 0.100 Uiso 1 1 calc R A 1
H57B H 0.8707 0.5223 0.2692 0.100 Uiso 1 1 calc R A 1
H57C H 0.7615 0.4960 0.2924 0.100 Uiso 1 1 calc R A 1
C58 C 0.6653(8) 0.7097(6) 0.0334(5) 0.060(2) Uiso 1 1 d . A 1
H58A H 0.6339 0.6791 0.0126 0.090 Uiso 1 1 calc R A 1
H58B H 0.7306 0.7182 -0.0007 0.090 Uiso 1 1 calc R A 1
H58C H 0.6138 0.7591 0.0418 0.090 Uiso 1 1 calc R A 1
C59 C 0.1001(8) 0.4885(5) 0.1489(5) 0.057(2) Uiso 1 1 d . A 1
H59A H 0.0601 0.4587 0.1348 0.086 Uiso 1 1 calc R A 1
H59B H 0.1654 0.4897 0.1114 0.086 Uiso 1 1 calc R A 1
H59C H 0.0556 0.5408 0.1535 0.086 Uiso 1 1 calc R A 1
C60 C 0.2470(9) 0.3290(6) 0.3953(6) 0.072(3) Uiso 1 1 d . A 1
H60A H 0.3242 0.3242 0.3852 0.107 Uiso 1 1 calc R A 1
H60B H 0.2344 0.2782 0.4016 0.107 Uiso 1 1 calc R A 1
H60C H 0.2124 0.3528 0.4402 0.107 Uiso 1 1 calc R A 1
N1 N -0.0628(5) 1.0527(3) 0.4116(4) 0.0461(16) Uani 1 1 d . . 1
N2 N 0.0281(5) 0.9538(4) 0.3265(4) 0.0474(16) Uani 1 1 d . A 1
N3 N 0.0861(5) 0.9089(3) 0.4441(4) 0.0464(17) Uani 1 1 d . A 1
N4 N 0.1810(5) 0.8285(3) 0.5383(4) 0.0442(16) Uani 1 1 d . A 1
O1 O -0.0852(5) 1.4512(3) 0.0206(3) 0.0503(14) Uani 1 1 d . A 1
O2 O 0.0274(5) 1.3398(3) -0.0597(3) 0.0579(16) Uani 1 1 d . A 1
O3 O -0.6473(4) 1.2255(3) 0.1355(3) 0.0515(14) Uani 1 1 d . A 1
O4 O -0.5240(4) 1.1214(3) 0.0489(3) 0.0524(14) Uani 1 1 d . A 1
O5 O 0.6911(5) 0.6698(3) 0.1017(3) 0.0586(16) Uani 1 1 d . A 1
O6 O 0.7545(4) 0.5912(3) 0.2209(3) 0.0524(15) Uani 1 1 d . A 1
O7 O 0.1283(5) 0.4535(3) 0.2182(3) 0.0488(13) Uani 1 1 d . A 1
O8 O 0.2019(5) 0.3767(3) 0.3338(3) 0.0501(14) Uani 1 1 d . A 1
Zn1 Zn 0.0000 1.0000 0.5000 0.0963(9) Uani 1 2 d S . 1
C61 C 0.0025(7) 0.3200(5) 0.3126(5) 0.053(2) Uani 1 1 d . B 1
H61 H 0.0561 0.3510 0.3011 0.064 Uiso 1 1 calc R B 1
Cl1 Cl -0.1027(2) 0.35557(16) 0.38587(15) 0.0811(9) Uani 1 1 d . B 1
Cl2 Cl 0.0671(2) 0.22270(14) 0.33800(17) 0.0743(8) Uani 1 1 d . B 1
Cl3 Cl -0.05287(19) 0.32946(14) 0.23248(14) 0.0632(7) Uani 1 1 d . B 1
C62 C 0.5410(11) 0.2444(7) 0.4970(8) 0.097(4) Uani 1 1 d . C 1
H62 H 0.6178 0.2219 0.5000 0.117 Uiso 1 1 calc R C 1
Cl4 Cl 0.5074(4) 0.1839(3) 0.4524(4) 0.151(2) Uani 1 1 d . C 1
Cl5 Cl 0.5332(2) 0.33586(17) 0.44404(18) 0.0864(9) Uani 1 1 d . C 1
Cl6 Cl 0.4690(5) 0.2557(4) 0.5863(3) 0.157(2) Uani 1 1 d . C 1
C63 C 0.2242(7) 0.1015(6) 0.1013(6) 0.069(3) Uani 1 1 d . D 1
H63 H 0.2923 0.1122 0.1039 0.082 Uiso 1 1 calc R D 1
Cl7 Cl 0.1134(2) 0.17967(19) 0.1337(2) 0.0910(10) Uani 1 1 d . D 1
Cl8 Cl 0.2137(3) 0.0141(2) 0.1572(2) 0.1158(13) Uani 1 1 d . D 1
Cl9 Cl 0.2286(2) 0.09489(18) 0.00924(18) 0.0871(9) Uani 1 1 d . D 1
C64 C 0.0063(9) 0.6188(9) 0.3771(8) 0.096(4) Uani 1 1 d . E 1
H64 H 0.0831 0.5999 0.3527 0.116 Uiso 1 1 calc R E 1
Cl10 Cl -0.0631(4) 0.6780(3) 0.3086(2) 0.1270(14) Uani 1 1 d . E 1
Cl11 Cl 0.0028(4) 0.6697(4) 0.4472(2) 0.1436(19) Uani 1 1 d . E 1
Cl12 Cl -0.0458(4) 0.5370(3) 0.4125(2) 0.1189(13) Uani 1 1 d . E 1
C65 C 0.5303(15) 0.8855(8) 0.2427(9) 0.078(5) Uani 0.678(5) 1 d P A 1
H65 H 0.5379 0.8949 0.2908 0.093 Uiso 0.678(5) 1 calc PR A 1
Cl13 Cl 0.5178(7) 0.9750(3) 0.1778(3) 0.136(3) Uani 0.678(5) 1 d P A 1
Cl14 Cl 0.6448(6) 0.8139(3) 0.2043(4) 0.147(3) Uani 0.678(5) 1 d P A 1
Cl15 Cl 0.4139(6) 0.8540(4) 0.2539(4) 0.134(3) Uani 0.678(5) 1 d P A 1
C66 C 0.784(2) 0.9276(11) 0.2851(10) 0.141(19) Uani 0.322(5) 1 d PDU A 1
H66 H 0.8370 0.9431 0.3044 0.170 Uiso 0.322(5) 1 calc PR A 1
Cl16 Cl 0.7315(18) 0.8577(10) 0.3497(9) 0.173(7) Uani 0.322(5) 1 d PDU A 1
Cl17 Cl 0.849(2) 0.8879(13) 0.2014(9) 0.217(10) Uani 0.322(5) 1 d PDU A 1
Cl18 Cl 0.677(3) 1.0087(12) 0.2687(17) 0.37(2) Uani 0.322(5) 1 d PDU A 1
C67 C 0.4637(11) 0.5485(11) 0.0332(12) 0.081(10) Uani 0.339(2) 1 d PD . 1
H67 H 0.4599 0.5483 0.0864 0.098 Uiso 0.339(2) 1 calc PR A 1
Cl19 Cl 0.3972(6) 0.6398(4) -0.0078(4) 0.071(2) Uani 0.339(2) 1 d PD A 1
Cl20 Cl 0.5987(3) 0.5255(2) -0.0174(2) 0.0729(12) Uani 0.678(5) 1 d PD . 1
O9 O 0.1568(10) 1.0615(7) 0.4485(6) 0.102(4) Uiso 0.816(16) 1 d P F 1
C68 C 0.2441(19) 1.0336(14) 0.3793(13) 0.061(6) Uiso 0.408(8) 1 d P F 1
H68A H 0.2111 1.0163 0.3474 0.092 Uiso 0.408(8) 1 calc PR F 1
H68B H 0.3013 0.9913 0.3951 0.092 Uiso 0.408(8) 1 calc PR F 1
H68C H 0.2742 1.0760 0.3525 0.092 Uiso 0.408(8) 1 calc PR F 1
C69 C 0.193(3) 1.0867(18) 0.4968(17) 0.087(8) Uiso 0.408(8) 1 d P F 1
H69A H 0.1333 1.1021 0.5380 0.131 Uiso 0.408(8) 1 calc PR F 1
H69B H 0.2209 1.1307 0.4728 0.131 Uiso 0.408(8) 1 calc PR F 1
H69C H 0.2494 1.0458 0.5146 0.131 Uiso 0.408(8) 1 calc PR F 1
C9B C -0.1868(6) 1.1571(4) 0.1057(4) 0.0418(17) Uiso 0.678(5) 1 d P A 2
C23B C -0.1141(7) 1.0899(5) 0.0611(4) 0.0450(18) Uiso 0.678(5) 1 d P A 2
H23C H -0.0380 1.0867 0.0586 0.054 Uiso 0.678(5) 1 calc PR A 2
H23D H -0.1259 1.1016 0.0104 0.054 Uiso 0.678(5) 1 calc PR A 2
C24B C -0.1371(12) 1.0089(9) 0.0959(8) 0.067(3) Uiso 0.678(5) 1 d P A 2
H24D H -0.0896 0.9695 0.0659 0.100 Uiso 0.678(5) 1 calc PR A 2
H24E H -0.2119 1.0112 0.0973 0.100 Uiso 0.678(5) 1 calc PR A 2
H24F H -0.1241 0.9963 0.1457 0.100 Uiso 0.678(5) 1 calc PR A 2
C39B C 0.2977(7) 0.6704(5) 0.2215(5) 0.0478(19) Uiso 0.322(5) 1 d P A 2
C53B C 0.2612(7) 0.7108(5) 0.1523(5) 0.051(2) Uiso 0.322(5) 1 d P A 2
H53C H 0.2745 0.7622 0.1427 0.061 Uiso 0.322(5) 1 calc PR A 2
H53D H 0.1828 0.7181 0.1612 0.061 Uiso 0.322(5) 1 calc PR A 2
C54B C 0.3184(18) 0.6676(13) 0.0751(12) 0.037(5) Uiso 0.322(5) 1 d P A 2
H54D H 0.2881 0.6990 0.0341 0.056 Uiso 0.322(5) 1 calc PR A 2
H54E H 0.3040 0.6172 0.0827 0.056 Uiso 0.322(5) 1 calc PR A 2
H54F H 0.3959 0.6616 0.0641 0.056 Uiso 0.322(5) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.042(4) 0.019(3) 0.070(4) 0.010(3) -0.020(3) 0.000(2)
N2 0.036(3) 0.037(3) 0.057(4) 0.006(3) -0.010(3) 0.002(3)
N3 0.029(3) 0.031(3) 0.072(5) -0.002(3) -0.008(3) -0.001(2)
N4 0.032(3) 0.024(3) 0.065(4) 0.003(3) -0.007(3) 0.002(2)
O1 0.056(3) 0.026(2) 0.063(3) 0.000(2) -0.008(3) -0.008(2)
O2 0.062(4) 0.048(3) 0.055(3) -0.004(3) 0.002(3) -0.015(3)
O3 0.022(3) 0.047(3) 0.080(4) -0.011(3) -0.008(2) -0.002(2)
O4 0.034(3) 0.048(3) 0.075(4) -0.009(3) -0.015(3) -0.007(2)
O5 0.047(3) 0.053(3) 0.056(3) 0.009(3) 0.001(3) -0.004(3)
O6 0.032(3) 0.053(3) 0.060(3) 0.008(3) -0.005(2) -0.006(2)
O7 0.056(3) 0.041(3) 0.058(3) -0.001(2) -0.026(3) -0.017(2)
O8 0.062(4) 0.035(3) 0.054(3) 0.009(2) -0.025(3) -0.012(2)
Zn1 0.1355(18) 0.0486(10) 0.0863(13) -0.0252(8) -0.0674(12) 0.0527(10)
C61 0.043(5) 0.053(5) 0.063(5) -0.001(4) -0.019(4) -0.011(4)
Cl1 0.0880(19) 0.0729(16) 0.0651(16) -0.0060(12) 0.0000(13) -0.0099(14)
Cl2 0.0572(14) 0.0534(13) 0.110(2) 0.0076(13) -0.0312(13) -0.0111(11)
Cl3 0.0573(14) 0.0648(14) 0.0727(15) -0.0058(11) -0.0232(11) -0.0171(11)
C62 0.083(8) 0.072(7) 0.136(11) -0.011(7) -0.053(8) 0.008(6)
Cl4 0.128(3) 0.093(3) 0.253(6) -0.039(3) -0.068(4) -0.027(2)
Cl5 0.0798(19) 0.0698(17) 0.103(2) -0.0134(15) -0.0343(16) 0.0058(13)
Cl6 0.177(5) 0.165(5) 0.139(4) 0.015(3) -0.024(3) -0.087(4)
C63 0.030(4) 0.061(6) 0.108(8) -0.008(5) -0.012(5) -0.005(4)
Cl7 0.0465(14) 0.094(2) 0.136(3) -0.0446(18) -0.0115(15) -0.0100(13)
Cl8 0.111(3) 0.094(2) 0.131(3) 0.026(2) -0.034(2) -0.030(2)
Cl9 0.0693(17) 0.0803(18) 0.100(2) -0.0122(15) -0.0232(15) 0.0044(14)
C64 0.053(6) 0.124(11) 0.114(10) -0.046(8) -0.020(6) -0.005(6)
Cl10 0.138(3) 0.117(3) 0.121(3) 0.009(2) -0.056(3) -0.016(2)
Cl11 0.126(3) 0.220(5) 0.116(3) -0.062(3) 0.004(2) -0.092(3)
Cl12 0.122(3) 0.138(3) 0.103(3) 0.013(2) -0.040(2) -0.046(3)
C65 0.109(13) 0.042(7) 0.076(10) -0.010(7) -0.006(9) -0.022(8)
Cl13 0.264(9) 0.094(4) 0.082(3) 0.027(3) -0.054(4) -0.102(5)
Cl14 0.145(5) 0.076(3) 0.192(6) -0.067(4) 0.070(5) -0.042(3)
Cl15 0.143(5) 0.101(4) 0.189(6) 0.037(4) -0.083(5) -0.075(4)
C66 0.14(2) 0.14(2) 0.15(2) -0.023(10) -0.040(10) -0.040(11)
Cl16 0.234(18) 0.132(11) 0.158(13) 0.011(10) -0.042(12) -0.074(11)
Cl17 0.29(2) 0.216(18) 0.176(15) -0.086(14) 0.012(14) -0.126(16)
Cl18 0.35(3) 0.41(3) 0.43(4) -0.06(3) -0.13(2) -0.17(3)
C67 0.10(3) 0.07(2) 0.055(17) -0.021(15) -0.016(16) 0.000(18)
Cl19 0.098(6) 0.057(4) 0.051(4) -0.011(3) -0.029(4) 0.006(4)
Cl20 0.062(2) 0.068(2) 0.093(3) -0.0053(19) -0.0214(19) -0.0224(17)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.352(10) . ?
C1 N1 1.387(11) . ?
C1 C2 1.468(11) . ?
C2 C5 1.371(11) . ?
C2 C3 1.407(10) . ?
C3 C8 1.403(11) . ?
C3 C4 1.430(11) 2_576 ?
C4 N1 1.350(10) 2_576 ?
C4 N4 1.379(10) . ?
C4 C3 1.430(11) 2_576 ?
C5 C6 1.392(11) . ?
C6 C7 1.433(10) . ?
C6 C9 1.551(11) . ?
C7 C8 1.355(11) . ?
C7 C10 1.558(11) . ?
C9 C18 1.529(11) . ?
C9 C11 1.536(10) . ?
C9 C23 1.541(10) . ?
C10 C17 1.542(11) . ?
C10 C12 1.544(11) . ?
C10 C25 1.569(11) . ?
C11 C12 1.403(11) . ?
C11 C16 1.406(11) . ?
C12 C13 1.353(11) . ?
C13 C14 1.398(11) . ?
C14 C15 1.378(11) . ?
C14 O1 1.396(9) . ?
C15 C16 1.374(11) . ?
C15 O2 1.378(10) . ?
C17 C18 1.382(11) . ?
C17 C22 1.398(11) . ?
C18 C19 1.405(11) . ?
C19 C20 1.384(11) . ?
C20 O4 1.378(10) . ?
C20 C21 1.387(11) . ?
C21 O3 1.376(10) . ?
C21 C22 1.398(12) . ?
C23 C24 1.65(3) . ?
C25 C26 1.522(12) . ?
C27 O1 1.435(10) . ?
C28 O2 1.406(10) . ?
C29 O3 1.460(10) . ?
C30 O4 1.401(11) . ?
C31 N2 1.321(10) . ?
C31 N3 1.359(11) . ?
C31 C32 1.470(11) . ?
C32 C33 1.386(11) . ?
C32 C35 1.395(12) . ?
C33 C38 1.376(11) . ?
C33 C34 1.478(11) . ?
C34 N4 1.311(10) . ?
C34 N3 1.367(10) . ?
C35 C36 1.387(12) . ?
C36 C37 1.427(11) . ?
C36 C39 1.539(11) . ?
C37 C38 1.397(11) . ?
C37 C40 1.529(10) . ?
C39 C53 1.475(12) . ?
C39 C47 1.568(11) . ?
C39 C41 1.573(12) . ?
C40 C48 1.526(11) . ?
C40 C55 1.546(11) . ?
C40 C42 1.556(10) . ?
C41 C46 1.394(11) . ?
C41 C42 1.430(11) . ?
C42 C43 1.317(11) . ?
C43 C44 1.401(11) . ?
C44 C45 1.366(12) . ?
C44 O6 1.384(9) . ?
C45 C46 1.372(11) . ?
C45 O5 1.380(10) . ?
C47 C52 1.394(11) . ?
C47 C48 1.405(11) . ?
C48 C49 1.374(10) . ?
C49 C50 1.408(11) . ?
C50 O8 1.359(9) . ?
C50 C51 1.409(11) . ?
C51 O7 1.367(10) . ?
C51 C52 1.370(11) . ?
C53 C54 1.49(3) . ?
C55 C56 1.528(11) . ?
C57 O6 1.417(11) . ?
C58 O5 1.408(11) . ?
C59 O7 1.415(11) . ?
C60 O8 1.442(12) . ?
N1 C4 1.350(10) 2_576 ?
N1 Zn1 1.983(7) . ?
N3 Zn1 2.008(6) . ?
Zn1 N1 1.983(7) 2_576 ?
Zn1 N3 2.008(6) 2_576 ?
C61 Cl1 1.742(9) . ?
C61 Cl2 1.744(9) . ?
C61 Cl3 1.780(9) . ?
C62 Cl4 1.700(15) . ?
C62 Cl6 1.709(16) . ?
C62 Cl5 1.745(14) . ?
C63 Cl9 1.729(12) . ?
C63 Cl8 1.739(11) . ?
C63 Cl7 1.771(9) . ?
C64 Cl11 1.720(14) . ?
C64 Cl12 1.754(16) . ?
C64 Cl10 1.762(15) . ?
C65 Cl15 1.727(19) . ?
C65 Cl14 1.761(16) . ?
C65 Cl13 1.818(15) . ?
C66 Cl16 1.742(10) . ?
C66 Cl18 1.749(10) . ?
C66 Cl17 1.750(10) . ?
C67 Cl20 1.748(10) . ?
C67 Cl19 1.754(10) . ?
C67 Cl20 1.86(3) 2_665 ?
Cl20 C67 1.86(3) 2_665 ?
O9 C69 1.32(3) . ?
O9 C68 1.54(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 N1 126.8(7) . . ?
N2 C1 C2 124.0(7) . . ?
N1 C1 C2 109.1(6) . . ?
C5 C2 C3 123.4(7) . . ?
C5 C2 C1 131.9(7) . . ?
C3 C2 C1 104.7(6) . . ?
C8 C3 C2 119.5(7) . . ?
C8 C3 C4 132.7(7) . 2_576 ?
C2 C3 C4 107.7(7) . 2_576 ?
N1 C4 N4 126.8(7) 2_576 . ?
N1 C4 C3 110.2(7) 2_576 2_576 ?
N4 C4 C3 123.0(7) . 2_576 ?
C2 C5 C6 116.6(7) . . ?
C5 C6 C7 120.7(7) . . ?
C5 C6 C9 124.6(7) . . ?
C7 C6 C9 114.7(6) . . ?
C8 C7 C6 121.6(7) . . ?
C8 C7 C10 126.3(7) . . ?
C6 C7 C10 112.0(6) . . ?
C7 C8 C3 118.2(7) . . ?
C18 C9 C11 104.4(6) . . ?
C18 C9 C23 115.6(6) . . ?
C11 C9 C23 114.3(6) . . ?
C18 C9 C6 104.3(6) . . ?
C11 C9 C6 103.5(6) . . ?
C23 C9 C6 113.4(6) . . ?
C17 C10 C12 106.2(6) . . ?
C17 C10 C7 104.7(6) . . ?
C12 C10 C7 103.7(6) . . ?
C17 C10 C25 115.4(6) . . ?
C12 C10 C25 114.3(6) . . ?
C7 C10 C25 111.5(6) . . ?
C12 C11 C16 118.7(7) . . ?
C12 C11 C9 115.4(6) . . ?
C16 C11 C9 125.6(6) . . ?
C13 C12 C11 120.8(7) . . ?
C13 C12 C10 125.9(7) . . ?
C11 C12 C10 113.0(7) . . ?
C12 C13 C14 119.8(7) . . ?
C15 C14 O1 115.7(7) . . ?
C15 C14 C13 120.6(7) . . ?
O1 C14 C13 123.6(7) . . ?
C16 C15 C14 119.8(7) . . ?
C16 C15 O2 123.7(7) . . ?
C14 C15 O2 116.5(7) . . ?
C15 C16 C11 120.2(7) . . ?
C18 C17 C22 120.7(7) . . ?
C18 C17 C10 114.3(7) . . ?
C22 C17 C10 124.9(7) . . ?
C17 C18 C19 119.3(7) . . ?
C17 C18 C9 115.1(7) . . ?
C19 C18 C9 125.6(6) . . ?
C20 C19 C18 120.2(7) . . ?
O4 C20 C19 122.5(7) . . ?
O4 C20 C21 117.3(7) . . ?
C19 C20 C21 120.1(7) . . ?
O3 C21 C20 115.3(7) . . ?
O3 C21 C22 124.5(7) . . ?
C20 C21 C22 120.2(8) . . ?
C17 C22 C21 119.2(7) . . ?
C9 C23 C24 117.2(13) . . ?
C26 C25 C10 116.2(7) . . ?
N2 C31 N3 129.0(7) . . ?
N2 C31 C32 123.5(7) . . ?
N3 C31 C32 107.4(7) . . ?
C33 C32 C35 119.6(7) . . ?
C33 C32 C31 108.1(7) . . ?
C35 C32 C31 132.2(8) . . ?
C38 C33 C32 123.1(7) . . ?
C38 C33 C34 131.2(7) . . ?
C32 C33 C34 105.6(6) . . ?
N4 C34 N3 128.4(7) . . ?
N4 C34 C33 123.3(7) . . ?
N3 C34 C33 108.3(7) . . ?
C36 C35 C32 119.0(8) . . ?
C35 C36 C37 120.2(7) . . ?
C35 C36 C39 125.2(8) . . ?
C37 C36 C39 114.6(7) . . ?
C38 C37 C36 120.2(7) . . ?
C38 C37 C40 125.9(7) . . ?
C36 C37 C40 113.8(6) . . ?
C33 C38 C37 117.6(7) . . ?
C53 C39 C36 115.9(7) . . ?
C53 C39 C47 114.4(7) . . ?
C36 C39 C47 104.1(6) . . ?
C53 C39 C41 115.1(6) . . ?
C36 C39 C41 102.9(6) . . ?
C47 C39 C41 102.8(6) . . ?
C48 C40 C37 106.9(6) . . ?
C48 C40 C55 113.3(6) . . ?
C37 C40 C55 114.0(6) . . ?
C48 C40 C42 106.3(6) . . ?
C37 C40 C42 103.7(6) . . ?
C55 C40 C42 111.9(6) . . ?
C46 C41 C42 117.6(7) . . ?
C46 C41 C39 126.5(7) . . ?
C42 C41 C39 115.8(6) . . ?
C43 C42 C41 121.4(7) . . ?
C43 C42 C40 127.0(7) . . ?
C41 C42 C40 111.6(6) . . ?
C42 C43 C44 120.4(7) . . ?
C45 C44 O6 116.2(6) . . ?
C45 C44 C43 119.5(7) . . ?
O6 C44 C43 124.3(7) . . ?
C44 C45 C46 121.1(7) . . ?
C44 C45 O5 116.3(7) . . ?
C46 C45 O5 122.7(7) . . ?
C45 C46 C41 119.9(7) . . ?
C52 C47 C48 120.6(7) . . ?
C52 C47 C39 124.3(7) . . ?
C48 C47 C39 115.1(7) . . ?
C49 C48 C47 119.2(7) . . ?
C49 C48 C40 127.0(7) . . ?
C47 C48 C40 113.8(6) . . ?
C48 C49 C50 120.4(7) . . ?
O8 C50 C49 124.8(7) . . ?
O8 C50 C51 115.4(7) . . ?
C49 C50 C51 119.8(7) . . ?
O7 C51 C52 125.2(7) . . ?
O7 C51 C50 115.2(7) . . ?
C52 C51 C50 119.5(8) . . ?
C51 C52 C47 120.4(8) . . ?
C39 C53 C54 118.3(13) . . ?
C56 C55 C40 116.6(6) . . ?
C4 N1 C1 108.1(6) 2_576 . ?
C4 N1 Zn1 126.0(6) 2_576 . ?
C1 N1 Zn1 125.8(5) . . ?
C31 N2 C1 123.6(7) . . ?
C31 N3 C34 110.5(6) . . ?
C31 N3 Zn1 124.9(5) . . ?
C34 N3 Zn1 124.6(6) . . ?
C34 N4 C4 123.9(6) . . ?
C14 O1 C27 117.0(6) . . ?
C15 O2 C28 119.1(6) . . ?
C21 O3 C29 116.4(6) . . ?
C20 O4 C30 118.9(6) . . ?
C45 O5 C58 120.3(7) . . ?
C44 O6 C57 116.8(6) . . ?
C51 O7 C59 116.9(6) . . ?
C50 O8 C60 117.5(7) . . ?
N1 Zn1 N1 180.000(1) 2_576 . ?
N1 Zn1 N3 90.1(3) 2_576 . ?
N1 Zn1 N3 89.9(3) . . ?
N1 Zn1 N3 89.9(3) 2_576 2_576 ?
N1 Zn1 N3 90.1(3) . 2_576 ?
N3 Zn1 N3 180.000(1) . 2_576 ?
Cl1 C61 Cl2 110.2(5) . . ?
Cl1 C61 Cl3 109.0(5) . . ?
Cl2 C61 Cl3 110.7(5) . . ?
Cl4 C62 Cl6 116.3(9) . . ?
Cl4 C62 Cl5 110.6(8) . . ?
Cl6 C62 Cl5 109.5(7) . . ?
Cl9 C63 Cl8 110.7(6) . . ?
Cl9 C63 Cl7 110.0(6) . . ?
Cl8 C63 Cl7 110.8(6) . . ?
Cl11 C64 Cl12 111.7(8) . . ?
Cl11 C64 Cl10 112.3(8) . . ?
Cl12 C64 Cl10 110.1(7) . . ?
Cl15 C65 Cl14 108.9(8) . . ?
Cl15 C65 Cl13 107.9(11) . . ?
Cl14 C65 Cl13 109.2(9) . . ?
Cl16 C66 Cl18 108.9(9) . . ?
Cl16 C66 Cl17 108.8(8) . . ?
Cl18 C66 Cl17 109.2(9) . . ?
Cl20 C67 Cl19 107.3(7) . . ?
Cl20 C67 Cl20 105.6(13) . 2_665 ?
Cl19 C67 Cl20 107.8(14) . 2_665 ?
C67 Cl20 C67 74.4(13) . 2_665 ?
C69 O9 C68 115.2(18) . . ?

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        25.94
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         2.052
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.189