Supplementary material for CrystEngComm
This journal is © The Royal Society of Chemistry 2003

data_global

_journal_coden_Cambridge         1350

loop_
_publ_author_name
'Israel Goldberg'
'Mikki Vinodu'

_publ_contact_author_name        'Prof Israel Goldberg'
_publ_contact_author_address     
;
School of Chemistry 
Tel-Aviv University 
Ramat-Aviv 
Tel-Aviv 
69978 
ISRAEL 
;

_publ_contact_author_email       GOLDBERG@POST.TAU.AC.IL

_publ_requested_journal          'Cryst Eng. Comm.'

_publ_section_title              
;
New crystal-engineering tool for the self-assembly
of porphyrin-based networks
;

data_Compound-2
_database_code_CSD               209223

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C45 H33 Cl2 N5 O3), 3/4(C2 H4 Cl2)'
_chemical_formula_sum            'C46.50 H36 Cl3.50 N5 O3'
_chemical_formula_weight         836.88

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.0600(2)
_cell_length_b                   15.0390(4)
_cell_length_c                   16.8170(6)
_cell_angle_alpha                83.7610(10)
_cell_angle_beta                 77.3240(11)
_cell_angle_gamma                88.522(2)
_cell_volume                     1976.99(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    6198
_cell_measurement_theta_min      1.94
_cell_measurement_theta_max      28.18

_exptl_crystal_description       prisms
_exptl_crystal_colour            drak-brown
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             867
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8839
_exptl_absorpt_correction_T_max  0.9541
_exptl_absorpt_process_details   '(Blessing, 1995)'

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      110(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  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi & Omega scans'
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9191
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         28.18
_reflns_number_total             9191
_reflns_number_gt                6198
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Nonius B.V.'
_computing_cell_refinement       Denzo
_computing_data_reduction        Denzo
_computing_structure_solution    SIR-92
_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. 

The structure contains molecules of dichloroethane as crystallization
solvent with partial occupancies.  These are located on, and disordered
about, the centers of inversion.
The two inner pyrrole H-atoms are disordered between the four N-pyrrole
sites.
;

_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^)+(0.0913P)^2^+2.3130P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9191
_refine_ls_number_parameters     573
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0661
_refine_ls_wR_factor_ref         0.1933
_refine_ls_wR_factor_gt          0.1686
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.167
_refine_ls_shift/su_mean         0.018

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
Cl1 Cl 0.09682(11) 0.58039(5) 0.06936(5) 0.0367(2) Uani 1 1 d . . .
Cl2 Cl 0.24663(13) 0.23122(7) 1.09100(6) 0.0570(3) Uani 1 1 d . . .
C1 C 0.5917(4) -0.13996(19) 0.60388(18) 0.0260(6) Uani 1 1 d . . .
C2 C 0.5525(4) -0.21357(19) 0.56214(18) 0.0269(6) Uani 1 1 d . . .
H2 H 0.4870 -0.2649 0.5867 0.032 Uiso 1 1 calc R . .
C3 C 0.6264(4) -0.19572(19) 0.48177(18) 0.0263(6) Uani 1 1 d . . .
H3 H 0.6225 -0.2323 0.4396 0.032 Uiso 1 1 calc R . .
C4 C 0.7120(4) -0.11096(19) 0.47178(18) 0.0256(6) Uani 1 1 d . . .
C5 C 0.8087(4) -0.06919(18) 0.39754(17) 0.0248(6) Uani 1 1 d . . .
C6 C 0.8734(4) 0.01858(19) 0.38725(17) 0.0257(6) Uani 1 1 d . . .
C7 C 0.9883(4) 0.0583(2) 0.31477(18) 0.0279(6) Uani 1 1 d . . .
H7 H 1.0390 0.0293 0.2679 0.033 Uiso 1 1 calc R . .
C8 C 1.0110(4) 0.1451(2) 0.32585(17) 0.0274(6) Uani 1 1 d . . .
H8 H 1.0795 0.1882 0.2881 0.033 Uiso 1 1 calc R . .
C9 C 0.9107(4) 0.15914(19) 0.40598(17) 0.0253(6) Uani 1 1 d . . .
C10 C 0.8956(3) 0.24070(19) 0.44045(17) 0.0251(6) Uani 1 1 d . . .
C11 C 0.8147(4) 0.25215(18) 0.52127(17) 0.0247(6) Uani 1 1 d . . .
C12 C 0.7939(4) 0.33606(19) 0.55656(18) 0.0284(6) Uani 1 1 d . . .
H12 H 0.8279 0.3933 0.5287 0.034 Uiso 1 1 calc R . .
C13 C 0.7169(4) 0.31824(19) 0.63673(18) 0.0276(6) Uani 1 1 d . . .
H13 H 0.6879 0.3606 0.6756 0.033 Uiso 1 1 calc R . .
C14 C 0.6872(4) 0.22325(18) 0.65224(17) 0.0248(6) Uani 1 1 d . . .
C15 C 0.6261(4) 0.17659(19) 0.73006(17) 0.0258(6) Uani 1 1 d . . .
C16 C 0.6083(4) 0.08257(19) 0.74593(17) 0.0263(6) Uani 1 1 d . . .
C17 C 0.5584(4) 0.0332(2) 0.82540(19) 0.0313(7) Uani 1 1 d . . .
H17 H 0.5429 0.0566 0.8768 0.038 Uiso 1 1 calc R . .
C18 C 0.5377(4) -0.0532(2) 0.81322(18) 0.0297(6) Uani 1 1 d . . .
H18 H 0.5069 -0.1018 0.8546 0.036 Uiso 1 1 calc R . .
C19 C 0.5709(4) -0.05769(19) 0.72624(17) 0.0262(6) Uani 1 1 d . . .
C20 C 0.5461(4) -0.13373(18) 0.68862(17) 0.0248(6) Uani 1 1 d . . .
N21 N 0.6850(3) -0.07823(16) 0.54648(14) 0.0251(5) Uani 1 1 d . . .
H21 H 0.7119 -0.0261 0.5576 0.027(17) Uiso 0.50 1 d PR . .
N22 N 0.8332(3) 0.08061(15) 0.44239(15) 0.0255(5) Uani 1 1 d . . .
H22 H 0.7750 0.0731 0.4909 0.017(15) Uiso 0.50 1 d PR . .
N23 N 0.7458(3) 0.18519(16) 0.58151(14) 0.0243(5) Uani 1 1 d . . .
H23 H 0.7530 0.1339 0.5681 0.04(2) Uiso 0.50 1 d PR . .
N24 N 0.6197(3) 0.02566(15) 0.68673(15) 0.0257(5) Uani 1 1 d . . .
H24 H 0.6555 0.0421 0.6306 0.05(2) Uiso 0.50 1 d PR . .
C25 C 0.4698(4) -0.21455(19) 0.74322(17) 0.0257(6) Uani 1 1 d . . .
C26 C 0.3161(4) -0.2106(2) 0.80090(17) 0.0273(6) Uani 1 1 d . . .
H26 H 0.2561 -0.1555 0.8051 0.033 Uiso 1 1 calc R . .
C27 C 0.2498(4) -0.2863(2) 0.85214(18) 0.0288(6) Uani 1 1 d . . .
H27 H 0.1467 -0.2821 0.8918 0.035 Uiso 1 1 calc R . .
C28 C 0.3339(4) -0.36746(19) 0.84541(17) 0.0273(6) Uani 1 1 d . . .
C29 C 0.4872(4) -0.3728(2) 0.78794(18) 0.0293(6) Uani 1 1 d . . .
H29 H 0.5457 -0.4283 0.7831 0.035 Uiso 1 1 calc R . .
C30 C 0.5533(4) -0.29699(19) 0.73820(18) 0.0280(6) Uani 1 1 d . . .
H30 H 0.6580 -0.3011 0.6996 0.034 Uiso 1 1 calc R . .
O31 O 0.2738(3) -0.44486(14) 0.89220(13) 0.0355(5) Uani 1 1 d . . .
H31 H 0.1976 -0.4325 0.9377 0.084(16) Uiso 1 1 d R . .
C32 C 0.8410(3) -0.11869(19) 0.32332(17) 0.0254(6) Uani 1 1 d . . .
C33 C 0.9167(3) -0.20312(19) 0.32126(18) 0.0258(6) Uani 1 1 d . . .
H33 H 0.9435 -0.2326 0.3698 0.031 Uiso 1 1 calc R . .
C34 C 0.9538(4) -0.2452(2) 0.24919(18) 0.0279(6) Uani 1 1 d . . .
H34 H 1.0073 -0.3022 0.2486 0.033 Uiso 1 1 calc R . .
C35 C 0.9122(4) -0.2032(2) 0.17852(18) 0.0303(6) Uani 1 1 d . . .
C36 C 0.8298(4) -0.1214(2) 0.18084(19) 0.0341(7) Uani 1 1 d . . .
H36 H 0.7957 -0.0940 0.1334 0.041 Uiso 1 1 calc R . .
C37 C 0.7968(4) -0.0792(2) 0.25184(18) 0.0302(6) Uani 1 1 d . . .
H37 H 0.7429 -0.0223 0.2519 0.036 Uiso 1 1 calc R . .
O38 O 0.9464(3) -0.23835(16) 0.10464(13) 0.0390(5) Uani 1 1 d . . .
H38 H 0.9971 -0.2994 0.1085 0.14(3) Uiso 1 1 d R . .
C39 C 0.9701(4) 0.32254(18) 0.38690(17) 0.0249(6) Uani 1 1 d . . .
C40 C 1.0932(4) 0.37337(19) 0.40827(18) 0.0284(6) Uani 1 1 d . . .
H40 H 1.1291 0.3566 0.4580 0.034 Uiso 1 1 calc R . .
C41 C 1.1635(4) 0.44815(19) 0.35751(18) 0.0287(6) Uani 1 1 d . . .
H41 H 1.2458 0.4827 0.3731 0.034 Uiso 1 1 calc R . .
C42 C 1.1140(4) 0.47294(19) 0.28371(18) 0.0283(6) Uani 1 1 d . . .
C43 C 0.9897(4) 0.4239(2) 0.26199(18) 0.0300(6) Uani 1 1 d . . .
H43 H 0.9535 0.4411 0.2125 0.036 Uiso 1 1 calc R . .
C44 C 0.9193(4) 0.34946(19) 0.31337(18) 0.0281(6) Uani 1 1 d . . .
H44 H 0.8347 0.3160 0.2983 0.034 Uiso 1 1 calc R . .
O45 O 1.1944(3) 0.54500(14) 0.23458(13) 0.0347(5) Uani 1 1 d . . .
H45 H 1.1592 0.5549 0.1813 0.072(14) Uiso 1 1 d R . .
C46 C 0.5740(4) 0.23132(19) 0.79984(17) 0.0262(6) Uani 1 1 d . . .
C47 C 0.6429(4) 0.2184(2) 0.86949(18) 0.0289(6) Uani 1 1 d . . .
H47 H 0.7291 0.1746 0.8724 0.035 Uiso 1 1 calc R . .
C48 C 0.5873(4) 0.2682(2) 0.93366(19) 0.0315(7) Uani 1 1 d . . .
H48 H 0.6341 0.2579 0.9810 0.038 Uiso 1 1 calc R . .
N49 N 0.4680(3) 0.33132(16) 0.93065(15) 0.0299(6) Uani 1 1 d . . .
C50 C 0.4006(4) 0.3479(2) 0.86361(19) 0.0309(6) Uani 1 1 d . . .
H50 H 0.3177 0.3937 0.8618 0.037 Uiso 1 1 calc R . .
C51 C 0.4512(4) 0.29892(19) 0.79816(18) 0.0283(6) Uani 1 1 d . . .
H51 H 0.4029 0.3109 0.7514 0.034 Uiso 1 1 calc R . .
C52 C 0.4042(5) 0.3808(2) 1.0026(2) 0.0411(8) Uani 1 1 d . . .
H52A H 0.3934 0.4450 0.9839 0.049 Uiso 1 1 calc R . .
H52B H 0.4878 0.3755 1.0382 0.049 Uiso 1 1 calc R . .
C53 C 0.2344(5) 0.3465(3) 1.0519(2) 0.0484(9) Uani 1 1 d . . .
H53A H 0.1499 0.3531 1.0169 0.058 Uiso 1 1 calc R . .
H53B H 0.1953 0.3829 1.0982 0.058 Uiso 1 1 calc R . .
Cl3A Cl 0.7518(14) 0.0495(8) 0.0069(7) 0.077(3) Uani 0.358(3) 1 d P . .
Cl3B Cl 0.7468(16) 0.0309(10) -0.0080(8) 0.113(5) Uani 0.358(3) 1 d P . .
C54 C 0.9607(10) 0.0402(4) 0.0189(4) 0.076(2) Uani 0.717(5) 1 d P . .
H54A H 1.0235 0.0951 -0.0077 0.092 Uiso 0.717(5) 1 d PR . .
H54B H 0.9586 0.0347 0.0783 0.092 Uiso 0.717(5) 1 d PR . .
Cl4 Cl 0.2853(3) 0.43544(15) 0.58329(18) 0.0933(7) Uani 0.70 1 d P . .
C55A C 0.452(2) 0.5069(10) 0.5487(12) 0.069(5) Uani 0.40 1 d P . .
C55B C 0.474(4) 0.4616(16) 0.4991(17) 0.101(11) Uani 0.30 1 d P . .

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
Cl1 0.0475(5) 0.0326(4) 0.0286(4) -0.0032(3) -0.0052(3) -0.0038(3)
Cl2 0.0526(6) 0.0592(6) 0.0514(6) 0.0099(5) -0.0026(4) 0.0042(5)
C1 0.0253(14) 0.0229(14) 0.0299(15) -0.0028(11) -0.0060(11) 0.0006(11)
C2 0.0268(14) 0.0222(14) 0.0318(15) -0.0037(11) -0.0063(11) -0.0019(11)
C3 0.0287(15) 0.0231(14) 0.0283(15) -0.0056(11) -0.0075(11) -0.0013(11)
C4 0.0256(14) 0.0229(14) 0.0297(15) -0.0053(11) -0.0084(11) 0.0018(11)
C5 0.0244(14) 0.0231(14) 0.0278(14) -0.0051(11) -0.0066(11) 0.0020(11)
C6 0.0258(14) 0.0250(14) 0.0275(14) -0.0046(11) -0.0078(11) 0.0009(11)
C7 0.0277(15) 0.0286(15) 0.0273(15) -0.0069(12) -0.0041(11) 0.0025(12)
C8 0.0263(14) 0.0285(15) 0.0262(14) -0.0021(11) -0.0029(11) -0.0017(11)
C9 0.0254(14) 0.0248(14) 0.0267(14) -0.0050(11) -0.0070(11) 0.0009(11)
C10 0.0235(14) 0.0245(14) 0.0279(14) -0.0033(11) -0.0068(11) -0.0010(11)
C11 0.0262(14) 0.0234(14) 0.0252(14) -0.0034(11) -0.0063(11) -0.0001(11)
C12 0.0322(15) 0.0218(14) 0.0304(15) -0.0040(11) -0.0049(12) 0.0021(12)
C13 0.0328(16) 0.0213(14) 0.0289(15) -0.0067(11) -0.0053(12) 0.0005(11)
C14 0.0247(14) 0.0235(14) 0.0280(14) -0.0063(11) -0.0075(11) -0.0005(11)
C15 0.0271(14) 0.0241(14) 0.0278(14) -0.0064(11) -0.0075(11) -0.0017(11)
C16 0.0270(14) 0.0262(14) 0.0277(15) -0.0055(11) -0.0092(11) 0.0009(11)
C17 0.0394(17) 0.0283(15) 0.0282(15) -0.0046(12) -0.0103(13) -0.0014(13)
C18 0.0369(17) 0.0259(15) 0.0275(15) -0.0020(12) -0.0098(12) -0.0004(12)
C19 0.0271(14) 0.0242(14) 0.0277(15) -0.0024(11) -0.0074(11) 0.0027(11)
C20 0.0247(14) 0.0233(14) 0.0265(14) -0.0021(11) -0.0063(11) 0.0028(11)
N21 0.0281(12) 0.0228(12) 0.0240(12) -0.0033(9) -0.0044(9) -0.0010(10)
N22 0.0275(12) 0.0230(12) 0.0259(13) -0.0048(9) -0.0045(10) -0.0010(9)
N23 0.0246(12) 0.0230(12) 0.0257(12) -0.0048(9) -0.0053(9) -0.0005(9)
N24 0.0267(12) 0.0219(12) 0.0285(13) -0.0031(10) -0.0060(10) -0.0006(9)
C25 0.0274(14) 0.0251(14) 0.0254(14) -0.0033(11) -0.0072(11) -0.0011(11)
C26 0.0295(15) 0.0262(14) 0.0279(15) -0.0057(11) -0.0089(11) 0.0033(12)
C27 0.0272(15) 0.0332(16) 0.0253(14) -0.0048(12) -0.0038(11) 0.0008(12)
C28 0.0318(15) 0.0253(14) 0.0243(14) 0.0006(11) -0.0059(11) -0.0038(12)
C29 0.0302(15) 0.0240(14) 0.0322(16) -0.0024(12) -0.0044(12) 0.0025(12)
C30 0.0267(15) 0.0268(15) 0.0284(15) -0.0046(12) -0.0011(11) 0.0005(12)
O31 0.0400(13) 0.0300(11) 0.0316(12) 0.0019(9) 0.0006(10) -0.0021(9)
C32 0.0233(14) 0.0279(14) 0.0261(14) -0.0064(11) -0.0061(11) -0.0005(11)
C33 0.0235(14) 0.0254(14) 0.0294(15) -0.0042(11) -0.0067(11) -0.0005(11)
C34 0.0245(14) 0.0255(14) 0.0354(16) -0.0078(12) -0.0079(12) 0.0019(11)
C35 0.0273(15) 0.0360(16) 0.0294(15) -0.0105(12) -0.0067(12) -0.0015(12)
C36 0.0361(17) 0.0389(17) 0.0298(16) -0.0058(13) -0.0121(13) 0.0057(14)
C37 0.0335(16) 0.0293(15) 0.0292(15) -0.0050(12) -0.0099(12) 0.0069(12)
O38 0.0460(14) 0.0440(14) 0.0298(12) -0.0152(10) -0.0099(10) 0.0073(11)
C39 0.0250(14) 0.0212(13) 0.0280(15) -0.0042(11) -0.0042(11) 0.0006(11)
C40 0.0328(16) 0.0245(14) 0.0277(15) -0.0047(11) -0.0054(12) 0.0009(12)
C41 0.0320(15) 0.0233(14) 0.0321(16) -0.0078(12) -0.0069(12) -0.0010(12)
C42 0.0317(16) 0.0208(14) 0.0303(15) -0.0037(11) -0.0019(12) 0.0006(11)
C43 0.0335(16) 0.0304(15) 0.0263(15) -0.0032(12) -0.0068(12) 0.0010(12)
C44 0.0300(15) 0.0263(14) 0.0283(15) -0.0034(11) -0.0066(12) -0.0033(12)
O45 0.0450(13) 0.0243(11) 0.0340(12) 0.0006(9) -0.0084(10) -0.0063(9)
C46 0.0258(14) 0.0244(14) 0.0280(15) -0.0035(11) -0.0038(11) -0.0065(11)
C47 0.0280(15) 0.0305(15) 0.0283(15) -0.0048(12) -0.0053(11) -0.0049(12)
C48 0.0327(16) 0.0337(16) 0.0294(15) -0.0050(12) -0.0079(12) -0.0070(13)
N49 0.0313(13) 0.0276(13) 0.0312(13) -0.0082(10) -0.0048(10) -0.0033(10)
C50 0.0308(16) 0.0276(15) 0.0346(16) -0.0052(12) -0.0067(12) -0.0023(12)
C51 0.0301(15) 0.0265(15) 0.0292(15) -0.0053(12) -0.0067(12) -0.0034(12)
C52 0.052(2) 0.0401(19) 0.0331(17) -0.0130(14) -0.0106(15) 0.0049(16)
C53 0.048(2) 0.052(2) 0.041(2) -0.0058(17) -0.0044(16) 0.0143(18)
Cl3A 0.058(5) 0.095(4) 0.053(3) 0.039(3) 0.012(3) 0.037(4)
Cl3B 0.053(5) 0.178(11) 0.096(8) 0.070(6) -0.029(5) -0.023(5)
C54 0.110(6) 0.063(4) 0.042(3) 0.007(3) 0.010(3) -0.014(4)
Cl4 0.0810(14) 0.0725(12) 0.143(2) -0.0409(14) -0.0483(15) 0.0140(10)
C55A 0.074(9) 0.041(7) 0.110(14) -0.006(8) -0.061(10) 0.010(6)
C55B 0.16(3) 0.079(15) 0.114(19) -0.069(14) -0.13(2) 0.085(16)

_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
Cl2 C53 1.795(4) . ?
C1 N21 1.372(4) . ?
C1 C20 1.404(4) . ?
C1 C2 1.450(4) . ?
C2 C3 1.353(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.441(4) . ?
C3 H3 0.9500 . ?
C4 N21 1.370(4) . ?
C4 C5 1.410(4) . ?
C5 C6 1.411(4) . ?
C5 C32 1.493(4) . ?
C6 N22 1.370(4) . ?
C6 C7 1.441(4) . ?
C7 C8 1.360(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.445(4) . ?
C8 H8 0.9500 . ?
C9 N22 1.368(4) . ?
C9 C10 1.404(4) . ?
C10 C11 1.399(4) . ?
C10 C39 1.499(4) . ?
C11 N23 1.382(4) . ?
C11 C12 1.442(4) . ?
C12 C13 1.356(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.441(4) . ?
C13 H13 0.9500 . ?
C14 N23 1.361(4) . ?
C14 C15 1.408(4) . ?
C15 C16 1.415(4) . ?
C15 C46 1.486(4) . ?
C16 N24 1.369(4) . ?
C16 C17 1.436(4) . ?
C17 C18 1.357(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.437(4) . ?
C18 H18 0.9500 . ?
C19 N24 1.378(4) . ?
C19 C20 1.404(4) . ?
C20 C25 1.499(4) . ?
N21 H21 0.8684 . ?
N22 H22 0.8448 . ?
N23 H23 0.8246 . ?
N24 H24 0.9326 . ?
C25 C30 1.397(4) . ?
C25 C26 1.401(4) . ?
C26 C27 1.392(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.385(4) . ?
C27 H27 0.9500 . ?
C28 O31 1.368(3) . ?
C28 C29 1.398(4) . ?
C29 C30 1.383(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
O31 H31 0.9042 . ?
C32 C37 1.395(4) . ?
C32 C33 1.395(4) . ?
C33 C34 1.398(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.387(4) . ?
C34 H34 0.9500 . ?
C35 O38 1.373(4) . ?
C35 C36 1.382(5) . ?
C36 C37 1.384(4) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
O38 H38 0.9966 . ?
C39 C40 1.398(4) . ?
C39 C44 1.402(4) . ?
C40 C41 1.388(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.396(4) . ?
C41 H41 0.9500 . ?
C42 O45 1.373(3) . ?
C42 C43 1.392(4) . ?
C43 C44 1.389(4) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
O45 H45 0.9927 . ?
C46 C47 1.396(4) . ?
C46 C51 1.403(4) . ?
C47 C48 1.369(4) . ?
C47 H47 0.9500 . ?
C48 N49 1.339(4) . ?
C48 H48 0.9500 . ?
N49 C50 1.353(4) . ?
N49 C52 1.479(4) . ?
C50 C51 1.373(4) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.507(5) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
Cl3A Cl3B 0.40(3) . ?
Cl3A C54 1.739(14) . ?
Cl3B C54 1.888(16) . ?
C54 C54 1.488(14) 2_755 ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
Cl4 C55A 1.699(16) . ?
Cl4 C55B 1.86(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N21 C1 C20 125.7(3) . . ?
N21 C1 C2 108.2(2) . . ?
C20 C1 C2 126.1(3) . . ?
C3 C2 C1 107.5(3) . . ?
C3 C2 H2 126.3 . . ?
C1 C2 H2 126.3 . . ?
C2 C3 C4 107.5(2) . . ?
C2 C3 H3 126.3 . . ?
C4 C3 H3 126.3 . . ?
N21 C4 C5 125.8(2) . . ?
N21 C4 C3 108.6(2) . . ?
C5 C4 C3 125.6(3) . . ?
C6 C5 C4 124.4(3) . . ?
C6 C5 C32 116.8(2) . . ?
C4 C5 C32 118.8(2) . . ?
N22 C6 C5 126.1(3) . . ?
N22 C6 C7 109.0(2) . . ?
C5 C6 C7 124.9(3) . . ?
C8 C7 C6 107.4(3) . . ?
C8 C7 H7 126.3 . . ?
C6 C7 H7 126.3 . . ?
C7 C8 C9 106.8(3) . . ?
C7 C8 H8 126.6 . . ?
C9 C8 H8 126.6 . . ?
N22 C9 C10 125.7(3) . . ?
N22 C9 C8 109.2(2) . . ?
C10 C9 C8 125.1(3) . . ?
C11 C10 C9 125.1(3) . . ?
C11 C10 C39 116.9(2) . . ?
C9 C10 C39 118.0(2) . . ?
N23 C11 C10 126.1(3) . . ?
N23 C11 C12 108.3(2) . . ?
C10 C11 C12 125.6(3) . . ?
C13 C12 C11 107.4(3) . . ?
C13 C12 H12 126.3 . . ?
C11 C12 H12 126.3 . . ?
C12 C13 C14 107.4(3) . . ?
C12 C13 H13 126.3 . . ?
C14 C13 H13 126.3 . . ?
N23 C14 C15 125.6(3) . . ?
N23 C14 C13 109.0(2) . . ?
C15 C14 C13 125.0(3) . . ?
C14 C15 C16 124.9(3) . . ?
C14 C15 C46 116.8(2) . . ?
C16 C15 C46 118.3(3) . . ?
N24 C16 C15 124.5(3) . . ?
N24 C16 C17 109.4(2) . . ?
C15 C16 C17 125.8(3) . . ?
C18 C17 C16 107.1(3) . . ?
C18 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
C17 C18 C19 107.4(3) . . ?
C17 C18 H18 126.3 . . ?
C19 C18 H18 126.3 . . ?
N24 C19 C20 126.1(3) . . ?
N24 C19 C18 108.9(2) . . ?
C20 C19 C18 124.9(3) . . ?
C1 C20 C19 124.6(3) . . ?
C1 C20 C25 117.9(2) . . ?
C19 C20 C25 117.5(2) . . ?
C4 N21 C1 108.2(2) . . ?
C4 N21 H21 128.4 . . ?
C1 N21 H21 123.2 . . ?
C9 N22 C6 107.5(2) . . ?
C9 N22 H22 124.5 . . ?
C6 N22 H22 127.9 . . ?
C14 N23 C11 107.9(2) . . ?
C14 N23 H23 135.7 . . ?
C11 N23 H23 116.4 . . ?
C16 N24 C19 107.1(2) . . ?
C16 N24 H24 124.8 . . ?
C19 N24 H24 128.1 . . ?
C30 C25 C26 117.8(3) . . ?
C30 C25 C20 120.1(3) . . ?
C26 C25 C20 122.1(3) . . ?
C27 C26 C25 121.0(3) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
O31 C28 C27 123.3(3) . . ?
O31 C28 C29 117.0(3) . . ?
C27 C28 C29 119.7(3) . . ?
C30 C29 C28 119.7(3) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C29 C30 C25 121.6(3) . . ?
C29 C30 H30 119.2 . . ?
C25 C30 H30 119.2 . . ?
C28 O31 H31 110.4 . . ?
C37 C32 C33 117.6(3) . . ?
C37 C32 C5 119.4(3) . . ?
C33 C32 C5 123.0(3) . . ?
C32 C33 C34 121.3(3) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
C35 C34 C33 119.7(3) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
O38 C35 C36 116.6(3) . . ?
O38 C35 C34 123.9(3) . . ?
C36 C35 C34 119.5(3) . . ?
C35 C36 C37 120.5(3) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
C36 C37 C32 121.3(3) . . ?
C36 C37 H37 119.3 . . ?
C32 C37 H37 119.3 . . ?
C35 O38 H38 112.2 . . ?
C40 C39 C44 118.2(3) . . ?
C40 C39 C10 121.1(3) . . ?
C44 C39 C10 120.7(2) . . ?
C41 C40 C39 120.6(3) . . ?
C41 C40 H40 119.7 . . ?
C39 C40 H40 119.7 . . ?
C40 C41 C42 120.4(3) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
O45 C42 C43 122.8(3) . . ?
O45 C42 C41 117.4(3) . . ?
C43 C42 C41 119.8(3) . . ?
C44 C43 C42 119.4(3) . . ?
C44 C43 H43 120.3 . . ?
C42 C43 H43 120.3 . . ?
C43 C44 C39 121.5(3) . . ?
C43 C44 H44 119.2 . . ?
C39 C44 H44 119.2 . . ?
C42 O45 H45 112.3 . . ?
C47 C46 C51 117.0(3) . . ?
C47 C46 C15 122.4(3) . . ?
C51 C46 C15 120.6(3) . . ?
C48 C47 C46 120.5(3) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
N49 C48 C47 121.0(3) . . ?
N49 C48 H48 119.5 . . ?
C47 C48 H48 119.5 . . ?
C48 N49 C50 120.7(3) . . ?
C48 N49 C52 119.6(3) . . ?
C50 N49 C52 119.6(3) . . ?
N49 C50 C51 120.4(3) . . ?
N49 C50 H50 119.8 . . ?
C51 C50 H50 119.8 . . ?
C50 C51 C46 120.4(3) . . ?
C50 C51 H51 119.8 . . ?
C46 C51 H51 119.8 . . ?
N49 C52 C53 112.3(3) . . ?
N49 C52 H52A 109.1 . . ?
C53 C52 H52A 109.1 . . ?
N49 C52 H52B 109.2 . . ?
C53 C52 H52B 109.1 . . ?
H52A C52 H52B 107.9 . . ?
C52 C53 Cl2 111.5(3) . . ?
C52 C53 H53A 109.3 . . ?
Cl2 C53 H53A 109.3 . . ?
C52 C53 H53B 109.3 . . ?
Cl2 C53 H53B 109.3 . . ?
H53A C53 H53B 108.0 . . ?
C54 C54 Cl3A 108.7(8) 2_755 . ?
C54 C54 Cl3B 96.9(8) 2_755 . ?
C54 C54 H54A 111.0 2_755 . ?
Cl3A C54 H54A 109.0 . . ?
Cl3B C54 H54A 113.3 . . ?
C54 C54 H54B 111.1 2_755 . ?
Cl3A C54 H54B 108.0 . . ?
Cl3B C54 H54B 115.1 . . ?
H54A C54 H54B 109.0 . . ?
C55A C55A Cl4 111.1(13) 2_666 . ?
C55B C55B Cl4 110(3) 2_666 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O31 H31 Cl1 0.90 2.21 3.067(2) 157.6 1_546
O38 H38 Cl1 1.00 2.07 3.020(3) 157.7 1_645
O45 H45 Cl1 0.99 2.05 3.039(2) 176.9 1_655

_diffrn_measured_fraction_theta_max 0.956
_diffrn_reflns_theta_full        28.18
_diffrn_measured_fraction_theta_full 0.956
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.074