# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        M.Hardie
_publ_contact_author_address     
;
School of Chemistry
University of Leeds
Woodhouse Lane
Leeds
LS2 9JT
UNITED KINGDOM
;

_publ_contact_author_email       M.J.HARDIE@LEEDS.AC.UK

_publ_section_title              
;
Extended 36 and 63 arrays of capsule motifs using
ligand tris{4-(3-pyridyl)phenylester}cyclotriguaiacylene
;
loop_
_publ_author_name
M.Hardie
'Tanya K. Ronson'

# Attachment 'complex1.CIF'

data_c_1:
_database_code_depnum_ccdc_archive 'CCDC 692044'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tris{4-(3-pyridyl)phenylester)cyclotriguaiacylene
;
_chemical_name_common            
tris(4-(3-pyridyl)phenylester)cyclotriguaiacylene
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62.50 H47.50 Cl7.50 N3 O9'
_chemical_formula_weight         1250.41

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           Hexagonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   16.6660(7)
_cell_length_b                   16.6660(7)
_cell_length_c                   38.157(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     9178.5(10)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8149
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      25.98

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3858
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8883
_exptl_absorpt_correction_T_max  0.9761
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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 X8 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38821
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         25.99
_reflns_number_total             4020
_reflns_number_gt                2701
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.1138P)^2^+38.8855P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4020
_refine_ls_number_parameters     259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.2310
_refine_ls_wR_factor_gt          0.1888
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
Cl1 Cl 0.06481(14) 0.94884(14) 0.05838(5) 0.1078(6) Uani 1 1 d . . .
O1 O 0.03651(15) 0.32191(14) 0.11022(6) 0.0340(6) Uani 1 1 d . . .
N1 N 0.2024(3) 0.8688(2) 0.02765(10) 0.0785(14) Uani 1 1 d . . .
C1 C -0.1159(2) -0.0206(2) 0.18630(8) 0.0288(7) Uani 1 1 d . . .
H1A H -0.0762 -0.0132 0.2068 0.035 Uiso 1 1 calc R . .
H1B H -0.1760 -0.0307 0.1953 0.035 Uiso 1 1 calc R . .
Cl2 Cl -0.1186(3) -0.0510(3) 0.28765(9) 0.1605(15) Uani 0.67 1 d P . .
O2 O 0.01622(15) 0.38888(15) 0.15875(6) 0.0344(6) Uani 1 1 d . . .
C2 C -0.0697(2) 0.0695(2) 0.16485(8) 0.0270(7) Uani 1 1 d . . .
Cl3 Cl 0.0000 0.0000 0.34582(19) 0.254(3) Uani 1 3 d S . .
O3 O -0.14545(16) 0.20042(16) 0.10696(6) 0.0375(6) Uani 1 1 d . . .
C3 C 0.0266(2) 0.1328(2) 0.16565(8) 0.0271(7) Uani 1 1 d . . .
Cl4 Cl 0.0000 0.0000 0.4294(5) 0.255(7) Uiso 0.50 3 d SP . .
C4 C 0.0605(2) 0.2168(2) 0.14718(8) 0.0287(7) Uani 1 1 d . . .
H4 H 0.1250 0.2604 0.1476 0.034 Uiso 1 1 calc R . .
Cl5 Cl -0.028(2) 0.0527(17) 0.4830(5) 0.346(11) Uiso 0.33 1 d P . .
C5 C 0.0021(2) 0.2370(2) 0.12860(8) 0.0294(7) Uani 1 1 d . . .
C6 C -0.0937(2) 0.1737(2) 0.12637(8) 0.0301(7) Uani 1 1 d . . .
C7 C -0.1281(2) 0.0900(2) 0.14483(8) 0.0293(7) Uani 1 1 d . . .
H7 H -0.1925 0.0460 0.1438 0.035 Uiso 1 1 calc R . .
C8 C 0.0332(2) 0.3922(2) 0.12786(9) 0.0288(7) Uani 1 1 d . . .
C9 C 0.0531(2) 0.4713(2) 0.10396(8) 0.0301(7) Uani 1 1 d . . .
C10 C 0.0582(2) 0.4647(2) 0.06782(9) 0.0381(8) Uani 1 1 d . . .
H10 H 0.0493 0.4088 0.0576 0.046 Uiso 1 1 calc R . .
C11 C 0.0765(3) 0.5400(2) 0.04652(9) 0.0412(8) Uani 1 1 d . . .
H11 H 0.0800 0.5350 0.0218 0.049 Uiso 1 1 calc R . .
C12 C 0.0897(2) 0.6232(2) 0.06102(9) 0.0345(7) Uani 1 1 d . . .
C13 C 0.0842(2) 0.6289(2) 0.09731(9) 0.0375(8) Uani 1 1 d . . .
H13 H 0.0935 0.6848 0.1076 0.045 Uiso 1 1 calc R . .
C14 C 0.0651(2) 0.5536(2) 0.11857(9) 0.0367(8) Uani 1 1 d . . .
H14 H 0.0602 0.5581 0.1432 0.044 Uiso 1 1 calc R . .
C15 C 0.1112(2) 0.7039(2) 0.03774(9) 0.0359(8) Uani 1 1 d . . .
C16 C 0.1761(3) 0.7937(3) 0.04755(11) 0.0633(13) Uani 1 1 d . . .
H16 H 0.2036 0.8024 0.0700 0.076 Uiso 1 1 calc R . .
C17 C 0.0954(3) 0.7710(3) -0.01572(11) 0.0513(10) Uani 1 1 d . . .
H17 H 0.0678 0.7643 -0.0381 0.062 Uiso 1 1 calc R . .
C18 C 0.1599(3) 0.8557(3) -0.00376(11) 0.0535(10) Uani 1 1 d . . .
H18 H 0.1760 0.9082 -0.0181 0.064 Uiso 1 1 calc R . .
C19 C 0.0705(3) 0.6944(3) 0.00526(11) 0.0519(10) Uani 1 1 d . . .
H19 H 0.0251 0.6347 -0.0027 0.062 Uiso 1 1 calc R . .
C20 C -0.2412(2) 0.1314(3) 0.10132(10) 0.0423(9) Uani 1 1 d . . .
H20A H -0.2446 0.0775 0.0895 0.063 Uiso 1 1 calc R . .
H20B H -0.2709 0.1574 0.0867 0.063 Uiso 1 1 calc R . .
H20C H -0.2732 0.1122 0.1239 0.063 Uiso 1 1 calc R . .
C21 C 0.0000 1.0000 0.0729(2) 0.097(3) Uani 1 3 d S . .
H21 H 0.0000 1.0000 0.0991 0.116 Uiso 1 3 calc SR . .
C22 C -0.0363(17) 0.0362(18) 0.3137(4) 0.109(7) Uani 0.33 1 d P . .
H22 H -0.0647 0.0717 0.3238 0.131 Uiso 0.33 1 calc PR . .
C23 C 0.0000 0.0000 0.4608(9) 0.122(9) Uiso 0.50 3 d SP . .

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 0.1208(14) 0.1304(15) 0.0916(11) -0.0055(10) -0.0264(10) 0.0772(12)
O1 0.0380(13) 0.0265(11) 0.0383(13) 0.0065(9) 0.0113(10) 0.0168(10)
N1 0.106(3) 0.0357(19) 0.060(2) 0.0088(17) -0.033(2) 0.010(2)
C1 0.0234(15) 0.0270(15) 0.0361(17) 0.0024(13) 0.0036(12) 0.0127(13)
Cl2 0.195(4) 0.202(4) 0.089(2) -0.014(2) 0.011(2) 0.103(3)
O2 0.0390(13) 0.0332(12) 0.0325(13) 0.0053(10) 0.0048(10) 0.0192(10)
C2 0.0269(15) 0.0243(15) 0.0308(16) -0.0002(12) 0.0044(12) 0.0135(12)
Cl3 0.293(6) 0.293(6) 0.178(6) 0.000 0.000 0.146(3)
O3 0.0347(12) 0.0378(13) 0.0435(13) 0.0085(10) 0.0009(10) 0.0208(11)
C3 0.0260(15) 0.0236(15) 0.0332(16) -0.0038(12) 0.0024(12) 0.0134(13)
C4 0.0237(15) 0.0246(15) 0.0369(17) -0.0020(13) 0.0053(13) 0.0114(12)
C5 0.0329(17) 0.0214(15) 0.0330(17) 0.0040(12) 0.0094(13) 0.0130(13)
C6 0.0302(16) 0.0303(16) 0.0332(17) 0.0018(13) 0.0041(13) 0.0178(14)
C7 0.0253(15) 0.0262(15) 0.0356(17) -0.0013(13) 0.0021(13) 0.0122(13)
C8 0.0216(14) 0.0255(15) 0.0384(18) 0.0017(13) 0.0014(13) 0.0110(12)
C9 0.0249(15) 0.0258(15) 0.0352(17) 0.0010(13) -0.0002(13) 0.0093(13)
C10 0.048(2) 0.0264(16) 0.0374(19) -0.0046(14) -0.0054(15) 0.0169(15)
C11 0.054(2) 0.0345(18) 0.0318(18) -0.0018(14) -0.0034(16) 0.0200(17)
C12 0.0328(17) 0.0280(16) 0.0370(18) 0.0014(13) -0.0052(14) 0.0110(14)
C13 0.047(2) 0.0296(17) 0.0379(19) 0.0003(14) 0.0005(15) 0.0204(15)
C14 0.0434(19) 0.0338(18) 0.0342(18) 0.0021(14) 0.0057(14) 0.0204(16)
C15 0.0371(18) 0.0318(17) 0.0367(18) 0.0034(14) -0.0034(14) 0.0157(15)
C16 0.088(3) 0.034(2) 0.046(2) 0.0043(17) -0.025(2) 0.013(2)
C17 0.056(2) 0.046(2) 0.044(2) 0.0060(17) -0.0149(18) 0.0196(19)
C18 0.063(3) 0.040(2) 0.048(2) 0.0111(17) -0.010(2) 0.0180(19)
C19 0.057(2) 0.0343(19) 0.052(2) 0.0007(17) -0.0195(19) 0.0134(18)
C20 0.0349(18) 0.047(2) 0.047(2) 0.0033(17) -0.0027(16) 0.0227(17)
C21 0.123(6) 0.123(6) 0.044(5) 0.000 0.000 0.062(3)
C22 0.16(2) 0.17(2) 0.047(9) 0.014(11) 0.006(11) 0.118(18)

_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
Cl1 C21 1.767(3) . ?
O1 C8 1.376(4) . ?
O1 C5 1.418(4) . ?
N1 C16 1.336(5) . ?
N1 C18 1.353(5) . ?
C1 C3 1.528(4) 2 ?
C1 C2 1.537(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
Cl2 C22 1.73(2) . ?
Cl2 C22 1.87(2) 2 ?
O2 C8 1.207(4) . ?
C2 C7 1.407(4) . ?
C2 C3 1.412(4) . ?
Cl3 C22 1.611(18) 2 ?
Cl3 C22 1.611(18) . ?
Cl3 C22 1.611(18) 3 ?
O3 C6 1.370(4) . ?
O3 C20 1.443(4) . ?
C3 C4 1.410(4) . ?
C3 C1 1.528(4) 3 ?
Cl4 C23 1.20(3) . ?
Cl4 Cl5 2.36(2) . ?
Cl4 Cl5 2.36(2) 3 ?
Cl4 Cl5 2.36(2) 2 ?
C4 C5 1.375(5) . ?
C4 H4 0.9500 . ?
Cl5 C23 1.45(2) . ?
Cl5 Cl5 1.75(3) 11_556 ?
Cl5 Cl5 1.75(3) 12_556 ?
Cl5 Cl5 2.04(3) 2 ?
Cl5 Cl5 2.04(3) 3 ?
C5 C6 1.409(4) . ?
C6 C7 1.404(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.497(4) . ?
C9 C10 1.389(5) . ?
C9 C14 1.399(5) . ?
C10 C11 1.396(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.403(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.394(5) . ?
C12 C15 1.498(5) . ?
C13 C14 1.391(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C19 1.383(5) . ?
C15 C16 1.390(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.357(6) . ?
C17 C19 1.383(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 Cl1 1.767(3) 3_465 ?
C21 Cl1 1.767(3) 2_675 ?
C21 H21 1.0000 . ?
C22 Cl2 1.87(2) 3 ?
C22 H22 1.0000 . ?
C23 Cl5 1.45(2) 2 ?
C23 Cl5 1.45(2) 3 ?

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
C8 O1 C5 116.1(2) . . ?
C16 N1 C18 116.8(4) . . ?
C3 C1 C2 114.0(2) 2 . ?
C3 C1 H1A 108.8 2 . ?
C2 C1 H1A 108.8 . . ?
C3 C1 H1B 108.8 2 . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C22 Cl2 C22 60.3(13) . 2 ?
C7 C2 C3 119.8(3) . . ?
C7 C2 C1 117.1(3) . . ?
C3 C2 C1 123.0(3) . . ?
C22 Cl3 C22 68.4(12) 2 . ?
C22 Cl3 C22 68.4(12) 2 3 ?
C22 Cl3 C22 68.4(12) . 3 ?
C6 O3 C20 116.5(3) . . ?
C4 C3 C2 118.2(3) . . ?
C4 C3 C1 118.4(3) . 3 ?
C2 C3 C1 123.4(3) . 3 ?
C23 Cl4 Cl5 29.9(5) . . ?
C23 Cl4 Cl5 29.9(5) . 3 ?
Cl5 Cl4 Cl5 51.2(8) . 3 ?
C23 Cl4 Cl5 29.9(5) . 2 ?
Cl5 Cl4 Cl5 51.2(8) . 2 ?
Cl5 Cl4 Cl5 51.2(8) 3 2 ?
C5 C4 C3 121.3(3) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C23 Cl5 Cl5 99.2(14) . 11_556 ?
C23 Cl5 Cl5 99.2(13) . 12_556 ?
Cl5 Cl5 Cl5 71.3(17) 11_556 12_556 ?
C23 Cl5 Cl5 45.4(10) . 2 ?
Cl5 Cl5 Cl5 90.000(4) 11_556 2 ?
Cl5 Cl5 Cl5 54.4(8) 12_556 2 ?
C23 Cl5 Cl5 45.4(10) . 3 ?
Cl5 Cl5 Cl5 54.4(8) 11_556 3 ?
Cl5 Cl5 Cl5 90.000(4) 12_556 3 ?
Cl5 Cl5 Cl5 60.000(4) 2 3 ?
C23 Cl5 Cl4 24.3(11) . . ?
Cl5 Cl5 Cl4 118.2(10) 11_556 . ?
Cl5 Cl5 Cl4 118.2(10) 12_556 . ?
Cl5 Cl5 Cl4 64.4(4) 2 . ?
Cl5 Cl5 Cl4 64.4(4) 3 . ?
C4 C5 C6 121.6(3) . . ?
C4 C5 O1 121.1(3) . . ?
C6 C5 O1 117.3(3) . . ?
O3 C6 C7 125.7(3) . . ?
O3 C6 C5 116.8(3) . . ?
C7 C6 C5 117.5(3) . . ?
C6 C7 C2 121.6(3) . . ?
C6 C7 H7 119.2 . . ?
C2 C7 H7 119.2 . . ?
O2 C8 O1 123.1(3) . . ?
O2 C8 C9 125.4(3) . . ?
O1 C8 C9 111.5(3) . . ?
C10 C9 C14 119.3(3) . . ?
C10 C9 C8 122.0(3) . . ?
C14 C9 C8 118.7(3) . . ?
C9 C10 C11 120.1(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 C12 121.0(3) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
C13 C12 C11 118.4(3) . . ?
C13 C12 C15 121.5(3) . . ?
C11 C12 C15 120.1(3) . . ?
C14 C13 C12 120.8(3) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C9 120.5(3) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
C19 C15 C16 115.9(3) . . ?
C19 C15 C12 123.0(3) . . ?
C16 C15 C12 121.0(3) . . ?
N1 C16 C15 124.8(4) . . ?
N1 C16 H16 117.6 . . ?
C15 C16 H16 117.6 . . ?
C18 C17 C19 118.8(4) . . ?
C18 C17 H17 120.6 . . ?
C19 C17 H17 120.6 . . ?
N1 C18 C17 123.0(4) . . ?
N1 C18 H18 118.5 . . ?
C17 C18 H18 118.5 . . ?
C15 C19 C17 120.6(3) . . ?
C15 C19 H19 119.7 . . ?
C17 C19 H19 119.7 . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Cl1 C21 Cl1 110.6(3) 3_465 2_675 ?
Cl1 C21 Cl1 110.6(3) 3_465 . ?
Cl1 C21 Cl1 110.6(3) 2_675 . ?
Cl1 C21 H21 108.3 3_465 . ?
Cl1 C21 H21 108.3 2_675 . ?
Cl1 C21 H21 108.3 . . ?
Cl3 C22 Cl2 114.3(14) . . ?
Cl3 C22 Cl2 107.3(13) . 3 ?
Cl2 C22 Cl2 111.4(9) . 3 ?
Cl3 C22 H22 107.9 . . ?
Cl2 C22 H22 107.9 . . ?
Cl2 C22 H22 107.9 3 . ?
Cl4 C23 Cl5 125.8(14) . . ?
Cl4 C23 Cl5 125.8(14) . 2 ?
Cl5 C23 Cl5 89.3(19) . 2 ?
Cl4 C23 Cl5 125.8(14) . 3 ?
Cl5 C23 Cl5 89.3(19) . 3 ?
Cl5 C23 Cl5 89.3(19) 2 3 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.696
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.075
# Attachment 'new_complex2.CIF'

data_c_2:
_database_code_depnum_ccdc_archive 'CCDC 692045'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tris(acetonitrile)chlorobis(tris{4-(3-pyridyl)phenylester)
cyclotriguaiacylene)-
trisilver(I) tetrafluoroborate acetonitrile clathrate
;
_chemical_name_common            
;
tris(acetonitrile)chlorobis(tris(4-(3-pyridyl)phenylester)
cyclotriguaiacylene)-trisilver(i) tetrafluoroborate acetonitrile
clathrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C132 H108 Ag3 B2 Cl F8 N12 O18'
_chemical_formula_weight         2682.98

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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           Hexagonal
_symmetry_space_group_name_H-M   P6(3)/m

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

_cell_length_a                   16.1966(4)
_cell_length_b                   16.1966(4)
_cell_length_c                   34.0682(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     7739.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2736
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8744
_exptl_absorpt_correction_T_max  0.9774
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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 X8 CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            145381
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         27.36
_reflns_number_total             5912
_reflns_number_gt                3897
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5912
_refine_ls_number_parameters     251
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0892
_refine_ls_wR_factor_ref         0.3413
_refine_ls_wR_factor_gt          0.2991
_refine_ls_goodness_of_fit_ref   1.319
_refine_ls_restrained_S_all      1.320
_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
Ag1 Ag 0.97981(5) 0.15544(5) 0.2500 0.0481(3) Uani 1 2 d S . .
Cl1 Cl 1.0000 0.0000 0.2500 0.0461(8) Uani 1 6 d S . .
O1 O 1.2985(3) -0.0413(3) 0.43247(11) 0.0376(9) Uani 1 1 d . . .
O2 O 1.3086(3) 0.0408(3) 0.48785(11) 0.0383(9) Uani 1 1 d . . .
O3 O 1.4867(3) 0.0230(3) 0.43123(12) 0.0428(9) Uani 1 1 d . . .
N1 N 1.0771(4) 0.2424(4) 0.30200(14) 0.0435(11) Uani 1 1 d . . .
C1 C 1.2360(4) -0.3116(4) 0.51954(15) 0.0320(11) Uani 1 1 d . . .
H1A H 1.2688 -0.3194 0.5425 0.038 Uiso 1 1 calc R . .
H1B H 1.1851 -0.3000 0.5295 0.038 Uiso 1 1 calc R . .
C2 C 1.3080(4) -0.2239(3) 0.49600(15) 0.0317(10) Uani 1 1 d . . .
C3 C 1.2732(4) -0.1729(4) 0.47451(15) 0.0331(11) Uani 1 1 d . . .
H3 H 1.2068 -0.1945 0.4745 0.040 Uiso 1 1 calc R . .
C4 C 1.3341(4) -0.0926(4) 0.45375(15) 0.0339(11) Uani 1 1 d . . .
C5 C 1.4326(4) -0.0585(4) 0.45240(15) 0.0337(11) Uani 1 1 d . . .
C6 C 1.4670(4) -0.1096(3) 0.47294(16) 0.0340(11) Uani 1 1 d . . .
H6 H 1.5329 -0.0898 0.4715 0.041 Uiso 1 1 calc R . .
C7 C 1.4061(3) -0.1902(3) 0.49578(14) 0.0297(10) Uani 1 1 d . . .
C8 C 1.2923(3) 0.0279(3) 0.45263(15) 0.0304(10) Uani 1 1 d . . .
C9 C 1.2641(4) 0.0840(4) 0.42747(15) 0.0353(11) Uani 1 1 d . . .
C10 C 1.2521(5) 0.0690(4) 0.38711(17) 0.0451(13) Uani 1 1 d . . .
H10 H 1.2616 0.0213 0.3752 0.054 Uiso 1 1 calc R . .
C11 C 1.2262(5) 0.1237(4) 0.36397(17) 0.0459(14) Uani 1 1 d . . .
H11 H 1.2192 0.1137 0.3364 0.055 Uiso 1 1 calc R . .
C12 C 1.2104(4) 0.1930(4) 0.38096(18) 0.0406(12) Uani 1 1 d . . .
C13 C 1.2224(5) 0.2078(4) 0.42185(18) 0.0444(14) Uani 1 1 d . . .
H13 H 1.2111 0.2542 0.4338 0.053 Uiso 1 1 calc R . .
C14 C 1.2505(4) 0.1556(4) 0.44469(18) 0.0434(13) Uani 1 1 d . . .
H14 H 1.2606 0.1679 0.4720 0.052 Uiso 1 1 calc R . .
C15 C 1.1757(4) 0.2459(4) 0.35639(17) 0.0414(12) Uani 1 1 d . . .
C16 C 1.2020(5) 0.3415(4) 0.3639(2) 0.0551(17) Uani 1 1 d . . .
H16 H 1.2438 0.3753 0.3850 0.066 Uiso 1 1 calc R . .
C17 C 1.1660(5) 0.3858(5) 0.3401(2) 0.0628(19) Uani 1 1 d . . .
H17 H 1.1829 0.4503 0.3446 0.075 Uiso 1 1 calc R . .
C18 C 1.1039(5) 0.3335(5) 0.30921(19) 0.0523(15) Uani 1 1 d . . .
H18 H 1.0801 0.3643 0.2928 0.063 Uiso 1 1 calc R . .
C19 C 1.1121(4) 0.1995(4) 0.32585(17) 0.0410(12) Uani 1 1 d . . .
H19 H 1.0919 0.1342 0.3214 0.049 Uiso 1 1 calc R . .
C20 C 1.5855(4) 0.0525(4) 0.4263(2) 0.0488(15) Uani 1 1 d . . .
H20A H 1.6160 0.0634 0.4521 0.073 Uiso 1 1 calc R . .
H20B H 1.6168 0.1117 0.4110 0.073 Uiso 1 1 calc R . .
H20C H 1.5913 0.0027 0.4124 0.073 Uiso 1 1 calc R . .
N2 N 0.8248(13) 0.0925(12) 0.2500 0.124(5) Uiso 1 2 d S . .
C22 C 0.741(2) 0.030(2) 0.2500 0.174(9) Uiso 1 2 d SD . .
C24 C 1.0000 0.0000 0.4298(8) 0.063(6) Uiso 0.50 3 d SPD . .
N3 N 1.0000 0.0000 0.4015(12) 0.117(10) Uiso 0.50 3 d SP . .
C23 C 1.0000 0.0000 0.4753(8) 0.121(14) Uiso 0.50 3 d SPD . .
N4 N 1.3333 0.6667 0.3991(6) 0.138(7) Uiso 1 3 d SD . .
C21 C 0.634(2) -0.043(3) 0.2500 0.238(16) Uiso 1 2 d SD . .
C25 C 1.3829(15) 0.7454(13) 0.3834(6) 0.062(5) Uiso 0.33 1 d PD . .
C26 C 1.441(3) 0.837(2) 0.3582(13) 0.140(14) Uiso 0.33 1 d PD . .

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
Ag1 0.0528(5) 0.0664(5) 0.0356(4) 0.000 0.000 0.0377(4)
Cl1 0.0408(11) 0.0408(11) 0.057(2) 0.000 0.000 0.0204(5)
O1 0.047(2) 0.0372(19) 0.0362(19) -0.0027(15) -0.0107(16) 0.0264(17)
O2 0.044(2) 0.0326(19) 0.039(2) -0.0016(15) -0.0034(16) 0.0196(17)
O3 0.045(2) 0.033(2) 0.051(2) 0.0044(17) 0.0021(18) 0.0206(18)
N1 0.056(3) 0.049(3) 0.038(2) 0.005(2) -0.004(2) 0.035(2)
C1 0.032(2) 0.031(2) 0.035(3) -0.003(2) 0.000(2) 0.017(2)
C2 0.031(2) 0.028(2) 0.038(3) -0.004(2) -0.001(2) 0.015(2)
C3 0.033(3) 0.032(3) 0.038(3) -0.008(2) -0.007(2) 0.019(2)
C4 0.040(3) 0.032(3) 0.036(2) -0.006(2) -0.008(2) 0.023(2)
C5 0.040(3) 0.026(2) 0.034(3) -0.0019(19) -0.001(2) 0.016(2)
C6 0.029(2) 0.025(2) 0.046(3) -0.003(2) -0.001(2) 0.012(2)
C7 0.029(2) 0.028(2) 0.036(2) -0.0053(19) -0.0053(19) 0.016(2)
C8 0.024(2) 0.027(2) 0.037(3) 0.0000(19) -0.0023(19) 0.0104(19)
C9 0.035(3) 0.033(3) 0.037(3) -0.004(2) -0.008(2) 0.017(2)
C10 0.057(4) 0.046(3) 0.044(3) -0.005(3) -0.009(3) 0.033(3)
C11 0.060(4) 0.054(4) 0.037(3) -0.004(3) -0.008(3) 0.038(3)
C12 0.046(3) 0.033(3) 0.046(3) -0.004(2) -0.010(3) 0.022(2)
C13 0.057(4) 0.036(3) 0.050(3) -0.008(2) -0.014(3) 0.031(3)
C14 0.056(4) 0.038(3) 0.043(3) -0.009(2) -0.017(3) 0.028(3)
C15 0.049(3) 0.038(3) 0.041(3) 0.003(2) -0.005(2) 0.025(3)
C16 0.062(4) 0.035(3) 0.067(4) -0.004(3) -0.022(3) 0.023(3)
C17 0.072(5) 0.035(3) 0.082(5) 0.003(3) -0.018(4) 0.027(3)
C18 0.062(4) 0.049(4) 0.051(3) 0.010(3) -0.004(3) 0.032(3)
C19 0.047(3) 0.041(3) 0.043(3) 0.002(2) 0.000(2) 0.028(3)
C20 0.044(3) 0.034(3) 0.062(4) 0.009(3) 0.015(3) 0.015(3)

_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
Ag1 N2 2.187(18) . ?
Ag1 N1 2.320(5) . ?
Ag1 N1 2.320(5) 10_556 ?
Ag1 Cl1 2.6961(7) . ?
Cl1 Ag1 2.6961(7) 3_645 ?
Cl1 Ag1 2.6961(7) 8_766 ?
O1 C8 1.362(6) . ?
O1 C4 1.423(6) . ?
O2 C8 1.224(6) . ?
O3 C5 1.369(6) . ?
O3 C20 1.433(7) . ?
N1 C18 1.336(8) . ?
N1 C19 1.364(7) . ?
C1 C7 1.525(7) 3_635 ?
C1 C2 1.537(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.399(7) . ?
C2 C3 1.415(7) . ?
C3 C4 1.372(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.404(7) . ?
C5 C6 1.395(7) . ?
C6 C7 1.412(7) . ?
C6 H6 0.9500 . ?
C7 C1 1.525(7) 5_865 ?
C8 C9 1.476(7) . ?
C9 C10 1.393(7) . ?
C9 C14 1.412(8) . ?
C10 C11 1.399(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.410(8) . ?
C12 C15 1.494(8) . ?
C13 C14 1.384(8) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C19 1.391(8) . ?
C15 C16 1.410(8) . ?
C16 C17 1.389(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.410(10) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
N2 C22 1.22(3) . ?
C22 C21 1.526(19) . ?
C24 N3 0.96(4) . ?
C24 C23 1.550(19) . ?
C23 C23 1.69(6) 7_756 ?
N4 C25 1.239(15) 3_755 ?
N4 C25 1.239(15) . ?
N4 C25 1.239(15) 5_775 ?
C25 C26 1.557(19) . ?
C25 C25 1.93(3) 3_755 ?
C25 C25 1.93(3) 5_775 ?

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 Ag1 N1 123.8(2) . . ?
N2 Ag1 N1 123.8(2) . 10_556 ?
N1 Ag1 N1 99.5(3) . 10_556 ?
N2 Ag1 Cl1 102.2(4) . . ?
N1 Ag1 Cl1 101.79(11) . . ?
N1 Ag1 Cl1 101.79(11) 10_556 . ?
Ag1 Cl1 Ag1 120.0 3_645 8_766 ?
Ag1 Cl1 Ag1 120.0 3_645 . ?
Ag1 Cl1 Ag1 120.0 8_766 . ?
C8 O1 C4 116.2(4) . . ?
C5 O3 C20 117.0(4) . . ?
C18 N1 C19 117.7(5) . . ?
C18 N1 Ag1 123.9(4) . . ?
C19 N1 Ag1 118.3(4) . . ?
C7 C1 C2 113.6(4) 3_635 . ?
C7 C1 H1A 108.9 3_635 . ?
C2 C1 H1A 108.9 . . ?
C7 C1 H1B 108.9 3_635 . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C7 C2 C3 118.4(5) . . ?
C7 C2 C1 123.6(4) . . ?
C3 C2 C1 118.0(4) . . ?
C4 C3 C2 120.9(5) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 121.8(5) . . ?
C3 C4 O1 120.4(5) . . ?
C5 C4 O1 117.8(5) . . ?
O3 C5 C6 125.7(5) . . ?
O3 C5 C4 116.8(5) . . ?
C6 C5 C4 117.6(5) . . ?
C5 C6 C7 121.5(5) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C2 C7 C6 119.7(4) . . ?
C2 C7 C1 123.2(5) . 5_865 ?
C6 C7 C1 117.1(4) . 5_865 ?
O2 C8 O1 122.4(4) . . ?
O2 C8 C9 124.9(5) . . ?
O1 C8 C9 112.7(4) . . ?
C10 C9 C14 119.2(5) . . ?
C10 C9 C8 121.7(5) . . ?
C14 C9 C8 119.1(5) . . ?
C9 C10 C11 120.4(5) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C12 C11 C10 120.7(5) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 118.8(5) . . ?
C11 C12 C15 120.1(5) . . ?
C13 C12 C15 121.0(5) . . ?
C14 C13 C12 120.7(5) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C9 120.2(5) . . ?
C13 C14 H14 119.9 . . ?
C9 C14 H14 119.9 . . ?
C19 C15 C16 117.7(5) . . ?
C19 C15 C12 119.9(5) . . ?
C16 C15 C12 122.4(5) . . ?
C17 C16 C15 119.2(6) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C16 C17 C18 118.8(6) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
N1 C18 C17 122.8(5) . . ?
N1 C18 H18 118.6 . . ?
C17 C18 H18 118.6 . . ?
N1 C19 C15 123.7(5) . . ?
N1 C19 H19 118.2 . . ?
C15 C19 H19 118.2 . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 N2 Ag1 158.1(18) . . ?
N2 C22 C21 176(3) . . ?
N3 C24 C23 180.000(9) . . ?
C24 C23 C23 180.000(9) . 7_756 ?
C25 N4 C25 102.6(18) 3_755 . ?
C25 N4 C25 102.6(18) 3_755 5_775 ?
C25 N4 C25 102.6(18) . 5_775 ?
N4 C25 C26 172(3) . . ?
N4 C25 C25 38.7(9) . 3_755 ?
C26 C25 C25 137(2) . 3_755 ?
N4 C25 C25 38.7(9) . 5_775 ?
C26 C25 C25 136(2) . 5_775 ?
C25 C25 C25 60.000(5) 3_755 5_775 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.36
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.129
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.179

# Attachment 'new_complex3.CIF'

data_c_3:
_database_code_depnum_ccdc_archive 'CCDC 692046'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tris(acetonitrile)chlorobis(tris{4-(3-pyridyl)phenylester)cyclotriguaiacylene)-
trisilver(I) hexafluoroarsenate
;
_chemical_name_common            
;
tris(acetonitrile)chlorobis(tris(4-(3-
pyridyl)phenylester)cyclotriguaiacylene)-trisilver(i) hexafluoroarsenate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C126 H99 Ag3 As2 Cl F12 N9 O18'
_chemical_formula_weight         2764.04

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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           Hexagonal
_symmetry_space_group_name_H-M   P6(3)/m

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

_cell_length_a                   15.7496(2)
_cell_length_b                   15.7496(2)
_cell_length_c                   35.0891(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     7537.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2788
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7720
_exptl_absorpt_correction_T_max  0.8756
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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 X8 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            85656
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         22.50
_reflns_number_total             3336
_reflns_number_gt                2570
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex 2'
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_reduction        'Bruker Apex 2'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour)'
_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.
AsF6 anions were very disordered. For one the As was located and refined
anisotropically. The three largest remaining
q peaks were assigned as partially occupied As atoms to account for charge
balance. Associated F positions were either not located or could not be
satistactorily refined, hence have been excluded. Remaining e-density
was too diffuse to adequately model solvent hence the SQUEEZE routine of
Platon was employed. R1~11.5% prior to this.
;

_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^)+(0.1587P)^2^+28.8828P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3336
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0959
_refine_ls_wR_factor_ref         0.2816
_refine_ls_wR_factor_gt          0.2630
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_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
Ag1 Ag 0.96795(8) 0.15439(9) 0.2500 0.0602(5) Uani 1 2 d S . .
Cl1 Cl 1.0000 0.0000 0.2500 0.0580(15) Uani 1 6 d S . .
OO1 O 1.3033(5) -0.0312(5) 0.43139(18) 0.0569(17) Uani 1 1 d . . .
OO2 O 1.2950(5) 0.0422(4) 0.48524(18) 0.0518(16) Uani 1 1 d . . .
OO3 O 1.4971(5) 0.0326(5) 0.42979(19) 0.0628(18) Uani 1 1 d . . .
NN1 N 1.0689(6) 0.2465(6) 0.3001(2) 0.058(2) Uani 1 1 d . . .
C1 C 1.2356(6) -0.3081(6) 0.5169(3) 0.047(2) Uani 1 1 d . . .
H1A H 1.1845 -0.2946 0.5266 0.056 Uiso 1 1 calc R . .
H1B H 1.2687 -0.3174 0.5392 0.056 Uiso 1 1 calc R . .
C2 C 1.3106(7) -0.2195(7) 0.4942(2) 0.049(2) Uani 1 1 d . . .
C3 C 1.2758(7) -0.1653(7) 0.4729(3) 0.050(2) Uani 1 1 d . . .
H3 H 1.2077 -0.1866 0.4728 0.060 Uiso 1 1 calc R . .
C4 C 1.3380(7) -0.0845(7) 0.4530(3) 0.050(2) Uani 1 1 d . . .
C5 C 1.4396(7) -0.0514(7) 0.4512(3) 0.054(2) Uani 1 1 d . . .
C6 C 1.4744(6) -0.1038(6) 0.4713(3) 0.047(2) Uani 1 1 d . . .
H6 H 1.5421 -0.0837 0.4702 0.057 Uiso 1 1 calc R . .
C7 C 1.4104(6) -0.1865(6) 0.4935(2) 0.043(2) Uani 1 1 d . . .
C8 C 1.2869(6) 0.0339(6) 0.4516(3) 0.046(2) Uani 1 1 d . . .
C9 C 1.2586(6) 0.0902(6) 0.4254(3) 0.051(2) Uani 1 1 d . . .
C10 C 1.2567(7) 0.0797(7) 0.3857(3) 0.053(2) Uani 1 1 d . . .
H10 H 1.2745 0.0361 0.3743 0.063 Uiso 1 1 calc R . .
C11 C 1.2280(7) 0.1348(7) 0.3627(3) 0.060(3) Uani 1 1 d . . .
H11 H 1.2268 0.1280 0.3358 0.072 Uiso 1 1 calc R . .
C12 C 1.2012(7) 0.1992(6) 0.3791(3) 0.054(2) Uani 1 1 d . . .
C13 C 1.2043(9) 0.2087(7) 0.4187(3) 0.066(3) Uani 1 1 d . . .
H13 H 1.1873 0.2529 0.4301 0.079 Uiso 1 1 calc R . .
C14 C 1.2318(8) 0.1551(7) 0.4417(3) 0.064(3) Uani 1 1 d . . .
H14 H 1.2325 0.1622 0.4686 0.077 Uiso 1 1 calc R . .
C15 C 1.1666(7) 0.2524(7) 0.3543(3) 0.057(3) Uani 1 1 d . . .
C16 C 1.1890(8) 0.3494(7) 0.3615(4) 0.076(3) Uani 1 1 d . . .
H16 H 1.2275 0.3843 0.3830 0.091 Uiso 1 1 calc R . .
C17 C 1.1536(10) 0.3928(9) 0.3367(4) 0.096(4) Uani 1 1 d . . .
H17 H 1.1705 0.4592 0.3404 0.116 Uiso 1 1 calc R . .
C18 C 1.0949(9) 0.3411(8) 0.3073(3) 0.072(3) Uani 1 1 d . . .
H18 H 1.0710 0.3724 0.2909 0.086 Uiso 1 1 calc R . .
C19 C 1.1061(7) 0.2041(7) 0.3228(3) 0.051(2) Uani 1 1 d . . .
H19 H 1.0910 0.1390 0.3173 0.061 Uiso 1 1 calc R . .
C20 C 1.5988(8) 0.0600(8) 0.4259(4) 0.075(3) Uani 1 1 d . . .
H20A H 1.6266 0.0626 0.4512 0.112 Uiso 1 1 calc R . .
H20B H 1.6349 0.1247 0.4138 0.112 Uiso 1 1 calc R . .
H20C H 1.6040 0.0115 0.4101 0.112 Uiso 1 1 calc R . .
NN2 N 0.8101(13) 0.0761(12) 0.2500 0.096(5) Uiso 1 2 d S . .
C22 C 0.730(2) 0.024(2) 0.2500 0.137(9) Uiso 1 2 d S . .
C21 C 0.621(3) -0.055(3) 0.2500 0.216(16) Uiso 1 2 d S . .
As1 As 0.3333 -0.3333 0.2500 0.0685(9) Uani 1 6 d S . .
As2 As 0.8065(7) 0.3250(7) 0.2261(3) 0.066(2) Uiso 0.12 1 d P . .
As3 As 0.913(2) 0.350(2) 0.2500 0.058(8) Uiso 0.04 2 d SP . .
As4 As 0.777(3) 0.272(3) 0.2500 0.079(10) Uiso 0.05 2 d SP . .

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
Ag1 0.0669(8) 0.0759(9) 0.0499(7) 0.000 0.000 0.0449(7)
Cl1 0.053(2) 0.053(2) 0.068(4) 0.000 0.000 0.0266(11)
OO1 0.070(4) 0.054(4) 0.058(4) -0.008(3) -0.021(3) 0.040(4)
OO2 0.059(4) 0.045(4) 0.045(4) 0.000(3) -0.003(3) 0.021(3)
OO3 0.066(5) 0.043(4) 0.071(4) 0.004(3) 0.006(4) 0.021(3)
NN1 0.080(6) 0.047(5) 0.051(5) 0.008(4) 0.002(4) 0.035(4)
C1 0.036(5) 0.046(5) 0.055(5) -0.006(4) 0.000(4) 0.017(4)
C2 0.067(7) 0.048(5) 0.038(5) -0.007(4) -0.002(4) 0.034(5)
C3 0.048(5) 0.046(6) 0.059(6) -0.013(5) -0.011(5) 0.026(5)
C4 0.053(6) 0.041(5) 0.054(5) -0.010(5) -0.015(5) 0.022(5)
C5 0.056(6) 0.037(5) 0.061(6) -0.009(5) 0.000(5) 0.017(5)
C6 0.039(5) 0.038(5) 0.063(6) -0.002(4) -0.004(4) 0.019(4)
C7 0.036(5) 0.041(5) 0.053(5) -0.013(4) -0.007(4) 0.019(4)
C8 0.041(5) 0.034(5) 0.053(6) 0.003(4) -0.003(4) 0.012(4)
C9 0.043(5) 0.039(5) 0.060(6) -0.003(4) -0.013(4) 0.012(4)
C10 0.049(6) 0.061(6) 0.052(6) -0.010(5) -0.002(5) 0.030(5)
C11 0.065(6) 0.070(7) 0.044(5) 0.006(5) -0.007(5) 0.034(6)
C12 0.061(6) 0.039(5) 0.065(7) -0.013(5) -0.014(5) 0.026(5)
C13 0.105(8) 0.056(6) 0.056(7) -0.018(5) -0.023(6) 0.055(6)
C14 0.108(9) 0.049(6) 0.048(6) -0.017(5) -0.013(5) 0.048(6)
C15 0.070(6) 0.046(6) 0.050(6) 0.000(4) -0.008(5) 0.025(5)
C16 0.081(8) 0.044(6) 0.093(8) -0.008(6) -0.025(7) 0.025(6)
C17 0.133(12) 0.054(7) 0.110(10) -0.003(7) -0.043(9) 0.053(8)
C18 0.097(9) 0.056(7) 0.064(7) 0.007(6) -0.014(6) 0.039(6)
C19 0.062(6) 0.047(5) 0.056(6) -0.006(4) -0.007(5) 0.037(5)
C20 0.065(7) 0.051(6) 0.094(9) 0.015(6) 0.018(6) 0.019(6)
As1 0.0499(10) 0.0499(10) 0.106(2) 0.000 0.000 0.0250(5)

_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
Ag1 NN2 2.152(18) . ?
Ag1 NN1 2.328(8) . ?
Ag1 NN1 2.328(8) 10_556 ?
Ag1 Cl1 2.7193(11) . ?
Cl1 Ag1 2.7193(11) 8_766 ?
Cl1 Ag1 2.7193(11) 3_645 ?
OO1 C8 1.373(11) . ?
OO1 C4 1.427(11) . ?
OO2 C8 1.186(10) . ?
OO3 C5 1.392(11) . ?
OO3 C20 1.441(12) . ?
NN1 C19 1.346(12) . ?
NN1 C18 1.357(13) . ?
C1 C2 1.527(13) . ?
C1 C7 1.534(12) 3_635 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.387(13) . ?
C2 C3 1.434(13) . ?
C3 C4 1.349(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.415(13) . ?
C5 C6 1.390(13) . ?
C6 C7 1.416(12) . ?
C6 H6 0.9500 . ?
C7 C1 1.534(12) 5_865 ?
C8 C9 1.493(13) . ?
C9 C10 1.403(13) . ?
C9 C14 1.408(13) . ?
C10 C11 1.412(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.403(13) . ?
C11 H11 0.9500 . ?
C12 C13 1.395(14) . ?
C12 C15 1.486(13) . ?
C13 C14 1.384(14) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.409(13) . ?
C15 C19 1.411(13) . ?
C16 C17 1.385(15) . ?
C16 H16 0.9500 . ?
C17 C18 1.354(16) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
NN2 C22 1.11(3) . ?
C22 C21 1.53(5) . ?
As2 As4 1.10(2) . ?
As2 As2 1.68(2) 10_556 ?
As2 As3 1.73(3) . ?
As3 As2 1.73(3) 10_556 ?
As3 As4 1.86(5) . ?
As4 As2 1.10(2) 10_556 ?

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
NN2 Ag1 NN1 126.2(3) . . ?
NN2 Ag1 NN1 126.2(3) . 10_556 ?
NN1 Ag1 NN1 98.1(4) . 10_556 ?
NN2 Ag1 Cl1 99.5(4) . . ?
NN1 Ag1 Cl1 100.54(19) . . ?
NN1 Ag1 Cl1 100.54(19) 10_556 . ?
Ag1 Cl1 Ag1 120.0 8_766 3_645 ?
Ag1 Cl1 Ag1 120.0 8_766 . ?
Ag1 Cl1 Ag1 120.0 3_645 . ?
C8 OO1 C4 115.8(7) . . ?
C5 OO3 C20 115.7(8) . . ?
C19 NN1 C18 117.9(9) . . ?
C19 NN1 Ag1 117.9(6) . . ?
C18 NN1 Ag1 124.1(6) . . ?
C2 C1 C7 113.2(7) . 3_635 ?
C2 C1 H1A 108.9 . . ?
C7 C1 H1A 108.9 3_635 . ?
C2 C1 H1B 108.9 . . ?
C7 C1 H1B 108.9 3_635 . ?
H1A C1 H1B 107.8 . . ?
C7 C2 C3 117.9(8) . . ?
C7 C2 C1 124.4(8) . . ?
C3 C2 C1 117.7(8) . . ?
C4 C3 C2 121.1(9) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 121.7(9) . . ?
C3 C4 OO1 121.2(8) . . ?
C5 C4 OO1 117.1(8) . . ?
C6 C5 OO3 125.2(8) . . ?
C6 C5 C4 117.9(8) . . ?
OO3 C5 C4 116.9(9) . . ?
C5 C6 C7 121.0(8) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C2 C7 C6 120.3(8) . . ?
C2 C7 C1 122.2(8) . 5_865 ?
C6 C7 C1 117.4(7) . 5_865 ?
OO2 C8 OO1 123.2(8) . . ?
OO2 C8 C9 126.5(9) . . ?
OO1 C8 C9 110.3(8) . . ?
C10 C9 C14 119.5(9) . . ?
C10 C9 C8 122.6(9) . . ?
C14 C9 C8 117.9(9) . . ?
C9 C10 C11 119.3(9) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C12 C11 C10 121.0(9) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C13 C12 C11 118.6(9) . . ?
C13 C12 C15 121.7(9) . . ?
C11 C12 C15 119.7(9) . . ?
C14 C13 C12 121.3(9) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C13 C14 C9 120.3(9) . . ?
C13 C14 H14 119.8 . . ?
C9 C14 H14 119.8 . . ?
C16 C15 C19 117.5(9) . . ?
C16 C15 C12 122.9(9) . . ?
C19 C15 C12 119.6(8) . . ?
C17 C16 C15 118.6(10) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C18 C17 C16 120.3(11) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 NN1 122.9(10) . . ?
C17 C18 H18 118.6 . . ?
NN1 C18 H18 118.6 . . ?
NN1 C19 C15 122.7(8) . . ?
NN1 C19 H19 118.6 . . ?
C15 C19 H19 118.6 . . ?
OO3 C20 H20A 109.5 . . ?
OO3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
OO3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 NN2 Ag1 169(2) . . ?
NN2 C22 C21 176(3) . . ?
As4 As2 As2 40.7(16) . 10_556 ?
As4 As2 As3 79(2) . . ?
As2 As2 As3 61.0(6) 10_556 . ?
As2 As3 As2 57.9(12) . 10_556 ?
As2 As3 As4 35.6(9) . . ?
As2 As3 As4 35.6(9) 10_556 . ?
As2 As4 As2 99(3) . 10_556 ?
As2 As4 As3 66(2) . . ?
As2 As4 As3 66(2) 10_556 . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        22.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.059
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.159

# Attachment 'new_complex4.CIF'

data_c_4:
_database_code_depnum_ccdc_archive 'CCDC 692047'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tris(acetonitrile)chlorobis(tris{4-(3-pyridyl)phenylester)cyclotriguaiacylene)-
trisilver(I) perchlorate acetonitrile clathrate
;
_chemical_name_common            
;
tris(acetonitrile)chlorobis(tris(4-(3-
pyridyl)phenylester)cyclotriguaiacylene)-trisilver(i) perchlorate
acetonitrile clathrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H102 Ag3 Cl3 N10 O26'
_chemical_formula_weight         2626.16

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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P6(3)/m

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

_cell_length_a                   16.2470(6)
_cell_length_b                   16.2470(6)
_cell_length_c                   34.382(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     7859.8(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9902
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      20.57

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2680
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8692
_exptl_absorpt_correction_T_max  0.9490
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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 X8 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            92000
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.18
_diffrn_reflns_theta_max         26.04
_reflns_number_total             5245
_reflns_number_gt                3614
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker APEX 2'
_computing_data_reduction        'Bruker APEX 2'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of 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.
Diffuse residual electron density could not be modelled as solvent or further
anion positions, hence the data was subjected to the SQUEEZE routine
;

_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^)+(0.1126P)^2^+2.6363P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5245
_refine_ls_number_parameters     256
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1986
_refine_ls_wR_factor_gt          0.1805
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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
Ag1 Ag -0.01999(4) -0.17551(4) 0.2500 0.0528(2) Uani 1 2 d S . .
Cl1 Cl 0.0000 0.0000 0.2500 0.0515(7) Uani 1 6 d S . .
O1 O 0.4879(2) 0.4645(2) 0.43108(8) 0.0444(7) Uani 1 1 d . . .
N1 N 0.0766(3) -0.1655(3) 0.30209(10) 0.0494(9) Uani 1 1 d . A .
C1 C 0.2359(3) 0.5469(3) 0.51919(12) 0.0359(9) Uani 1 1 d . . .
H1A H 0.1853 0.4848 0.5291 0.043 Uiso 1 1 calc R . .
H1B H 0.2686 0.5876 0.5419 0.043 Uiso 1 1 calc R . .
Cl2 Cl -0.3333 -0.6667 0.3602(2) 0.114(2) Uiso 0.50 3 d SPD . .
O2 O 0.2990(2) 0.33950(19) 0.43241(8) 0.0422(7) Uani 1 1 d . . .
N2 N -0.1795(10) -0.2619(9) 0.2500 0.098(4) Uiso 0.70 2 d SPD A 1
C2 C 0.3079(3) 0.5311(3) 0.49595(11) 0.0329(9) Uani 1 1 d . . .
O3 O 0.3076(2) 0.2669(2) 0.48755(8) 0.0414(7) Uani 1 1 d . . .
N3 N -0.171(4) -0.310(4) 0.2500 0.183(12) Uiso 0.30 2 d SPD A 2
C3 C 0.2739(3) 0.4467(3) 0.47460(11) 0.0359(9) Uani 1 1 d . . .
H3 H 0.2077 0.4021 0.4744 0.043 Uiso 1 1 calc R . .
N4 N 0.0000 0.0000 0.3976(6) 0.120(7) Uiso 0.50 3 d SPD . .
C4 C 0.3355(3) 0.4271(3) 0.45371(12) 0.0378(9) Uani 1 1 d . . .
O5 O -0.4208(13) -0.7105(15) 0.3741(5) 0.236(8) Uiso 0.50 1 d PD . .
C5 C 0.4331(3) 0.4915(3) 0.45194(11) 0.0363(9) Uani 1 1 d . . .
O6 O -0.3333 -0.6667 0.3211(7) 0.239(14) Uiso 0.50 3 d SPD . .
C6 C 0.4677(3) 0.5765(3) 0.47344(12) 0.0354(9) Uani 1 1 d . . .
H6 H 0.5338 0.6213 0.4730 0.043 Uiso 1 1 calc R . .
C7 C 0.4069(3) 0.5966(3) 0.49552(11) 0.0333(9) Uani 1 1 d . . .
C8 C 0.2922(3) 0.2639(3) 0.45295(13) 0.0365(9) Uani 1 1 d . . .
C9 C 0.2641(3) 0.1794(3) 0.42712(12) 0.0378(9) Uani 1 1 d . . .
C10 C 0.2537(3) 0.1831(3) 0.38661(13) 0.0442(10) Uani 1 1 d . . .
H10 H 0.2650 0.2405 0.3746 0.053 Uiso 1 1 calc R . .
C11 C 0.2265(4) 0.1021(3) 0.36442(13) 0.0504(12) Uani 1 1 d . . .
H11 H 0.2197 0.1050 0.3371 0.060 Uiso 1 1 calc R . .
C12 C 0.2089(3) 0.0166(3) 0.38102(13) 0.0422(10) Uani 1 1 d . . .
C13 C 0.2219(4) 0.0148(3) 0.42166(14) 0.0501(12) Uani 1 1 d . . .
H13 H 0.2116 -0.0423 0.4337 0.060 Uiso 1 1 calc R . .
C14 C 0.2493(3) 0.0944(3) 0.44373(13) 0.0470(11) Uani 1 1 d . . .
H14 H 0.2585 0.0920 0.4709 0.056 Uiso 1 1 calc R . .
C15 C 0.1742(3) -0.0711(3) 0.35609(13) 0.0431(10) Uani 1 1 d . A .
C16 C 0.1127(3) -0.0880(3) 0.32584(13) 0.0457(11) Uani 1 1 d . . .
H16 H 0.0939 -0.0422 0.3211 0.055 Uiso 1 1 calc R A .
C17 C 0.1044(4) -0.2296(4) 0.30930(15) 0.0606(13) Uani 1 1 d . . .
H17 H 0.0812 -0.2837 0.2929 0.073 Uiso 1 1 calc R A .
C18 C 0.1659(4) -0.2204(4) 0.33988(16) 0.0696(16) Uani 1 1 d . A .
H18 H 0.1832 -0.2675 0.3443 0.084 Uiso 1 1 calc R . .
C19 C 0.2008(4) -0.1401(4) 0.36354(16) 0.0611(14) Uani 1 1 d . . .
H19 H 0.2422 -0.1319 0.3846 0.073 Uiso 1 1 calc R A .
C20 C 0.5872(3) 0.5343(3) 0.42633(14) 0.0530(12) Uani 1 1 d . . .
H20A H 0.5931 0.5893 0.4122 0.079 Uiso 1 1 calc R . .
H20B H 0.6189 0.5063 0.4116 0.079 Uiso 1 1 calc R . .
H20C H 0.6171 0.5547 0.4519 0.079 Uiso 1 1 calc R . .
C21 C -0.2578(14) -0.2781(15) 0.2500 0.148(7) Uiso 0.70 2 d SPD A 1
C22 C -0.3617(14) -0.316(2) 0.2500 0.201(11) Uiso 0.70 2 d SPD A 1
C23 C -0.228(4) -0.390(4) 0.2500 0.183(12) Uiso 0.30 2 d SPD A 2
C24 C -0.274(4) -0.495(4) 0.2500 0.183(12) Uiso 0.30 2 d SPD A 2
C25 C 0.0000 0.0000 0.4300(5) 0.073(5) Uiso 0.50 3 d SPD . .
C26 C 0.0000 0.0000 0.4726(6) 0.128(10) Uiso 0.50 3 d SPD . .

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
Ag1 0.0582(4) 0.0452(3) 0.0431(3) 0.000 0.000 0.0168(3)
Cl1 0.0441(9) 0.0441(9) 0.0663(18) 0.000 0.000 0.0220(5)
O1 0.0448(17) 0.0403(17) 0.0544(18) -0.0025(13) 0.0031(14) 0.0260(15)
N1 0.063(3) 0.042(2) 0.046(2) -0.0082(17) -0.0031(18) 0.0283(19)
C1 0.031(2) 0.029(2) 0.045(2) 0.0058(17) -0.0003(18) 0.0134(17)
O2 0.0529(18) 0.0324(15) 0.0436(16) -0.0076(12) -0.0119(13) 0.0230(14)
C2 0.032(2) 0.031(2) 0.038(2) 0.0047(17) -0.0032(17) 0.0176(18)
O3 0.0461(17) 0.0392(16) 0.0418(18) -0.0026(13) -0.0039(13) 0.0235(14)
C3 0.032(2) 0.029(2) 0.047(2) 0.0012(18) -0.0074(18) 0.0148(18)
C4 0.043(2) 0.029(2) 0.042(2) -0.0023(17) -0.0085(19) 0.0184(19)
C5 0.043(2) 0.038(2) 0.038(2) 0.0026(17) -0.0055(18) 0.027(2)
C6 0.030(2) 0.031(2) 0.045(2) 0.0036(18) -0.0029(18) 0.0154(17)
C7 0.036(2) 0.026(2) 0.042(2) 0.0019(17) -0.0027(17) 0.0179(18)
C8 0.028(2) 0.037(2) 0.048(3) -0.0050(19) -0.0048(18) 0.0197(18)
C9 0.034(2) 0.035(2) 0.048(2) -0.0036(18) -0.0068(18) 0.0201(19)
C10 0.051(3) 0.034(2) 0.048(3) 0.0022(19) -0.003(2) 0.021(2)
C11 0.070(3) 0.043(3) 0.043(2) -0.003(2) -0.003(2) 0.031(3)
C12 0.047(3) 0.035(2) 0.049(3) -0.0112(19) -0.009(2) 0.024(2)
C13 0.064(3) 0.042(3) 0.057(3) -0.004(2) -0.016(2) 0.036(2)
C14 0.062(3) 0.043(3) 0.043(2) -0.005(2) -0.016(2) 0.032(2)
C15 0.046(2) 0.041(2) 0.049(3) -0.0064(19) -0.007(2) 0.026(2)
C16 0.059(3) 0.037(2) 0.046(2) -0.003(2) 0.000(2) 0.027(2)
C17 0.074(4) 0.053(3) 0.060(3) -0.018(3) -0.010(3) 0.035(3)
C18 0.078(4) 0.060(3) 0.091(4) -0.023(3) -0.020(3) 0.050(3)
C19 0.066(3) 0.055(3) 0.073(3) -0.021(3) -0.023(3) 0.037(3)
C20 0.055(3) 0.055(3) 0.060(3) 0.003(2) 0.010(2) 0.035(3)

_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
Ag1 N2 2.247(14) . ?
Ag1 N1 2.333(4) . ?
Ag1 N1 2.333(4) 10_556 ?
Ag1 N3 2.34(5) . ?
Ag1 Cl1 2.7038(5) . ?
Cl1 Ag1 2.7038(6) 3 ?
Cl1 Ag1 2.7038(5) 8_556 ?
O1 C5 1.375(5) . ?
O1 C20 1.445(6) . ?
N1 C17 1.348(6) . ?
N1 C16 1.364(5) . ?
C1 C7 1.533(5) 5_565 ?
C1 C2 1.540(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
Cl2 O5 1.321(17) 3_445 ?
Cl2 O5 1.321(17) 5_545 ?
Cl2 O5 1.321(17) . ?
Cl2 O6 1.35(2) . ?
O2 C8 1.372(5) . ?
O2 C4 1.439(5) . ?
N2 C21 1.163(14) . ?
C2 C3 1.403(5) . ?
C2 C7 1.418(5) . ?
O3 C8 1.212(5) . ?
N3 C23 1.155(18) . ?
C3 C4 1.392(6) . ?
C3 H3 0.9500 . ?
N4 C25 1.115(14) . ?
C4 C5 1.397(6) . ?
C5 C6 1.412(6) . ?
C6 C7 1.408(5) . ?
C6 H6 0.9500 . ?
C7 C1 1.533(5) 3_665 ?
C8 C9 1.502(6) . ?
C9 C14 1.399(6) . ?
C9 C10 1.408(6) . ?
C10 C11 1.389(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.416(6) . ?
C12 C15 1.510(6) . ?
C13 C14 1.369(6) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.371(6) . ?
C15 C19 1.411(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.406(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.395(6) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.479(15) . ?
C23 C24 1.478(18) . ?
C25 C26 1.464(15) . ?
C26 C26 1.89(4) 7_556 ?

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 Ag1 N1 124.69(16) . . ?
N2 Ag1 N1 124.69(16) . 10_556 ?
N1 Ag1 N1 100.29(19) . 10_556 ?
N2 Ag1 N3 21.6(12) . . ?
N1 Ag1 N3 114.9(7) . . ?
N1 Ag1 N3 114.9(7) 10_556 . ?
N2 Ag1 Cl1 98.7(4) . . ?
N1 Ag1 Cl1 101.83(9) . . ?
N1 Ag1 Cl1 101.83(9) 10_556 . ?
N3 Ag1 Cl1 120.3(13) . . ?
Ag1 Cl1 Ag1 120.0 3 8_556 ?
Ag1 Cl1 Ag1 120.0 3 . ?
Ag1 Cl1 Ag1 120.0 8_556 . ?
C5 O1 C20 117.1(3) . . ?
C17 N1 C16 116.6(4) . . ?
C17 N1 Ag1 124.1(3) . . ?
C16 N1 Ag1 119.2(3) . . ?
C7 C1 C2 113.8(3) 5_565 . ?
C7 C1 H1A 108.8 5_565 . ?
C2 C1 H1A 108.8 . . ?
C7 C1 H1B 108.8 5_565 . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
O5 Cl2 O5 107.6(10) 3_445 5_545 ?
O5 Cl2 O5 107.6(10) 3_445 . ?
O5 Cl2 O5 107.6(10) 5_545 . ?
O5 Cl2 O6 111.2(9) 3_445 . ?
O5 Cl2 O6 111.2(9) 5_545 . ?
O5 Cl2 O6 111.2(9) . . ?
C8 O2 C4 115.6(3) . . ?
C21 N2 Ag1 158.6(15) . . ?
C3 C2 C7 118.2(4) . . ?
C3 C2 C1 118.2(3) . . ?
C7 C2 C1 123.5(3) . . ?
C23 N3 Ag1 158(5) . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 121.9(4) . . ?
C3 C4 O2 120.1(4) . . ?
C5 C4 O2 118.0(4) . . ?
O1 C5 C4 117.3(4) . . ?
O1 C5 C6 125.5(4) . . ?
C4 C5 C6 117.2(4) . . ?
C7 C6 C5 121.8(4) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C6 C7 C2 119.7(4) . . ?
C6 C7 C1 117.2(3) . 3_665 ?
C2 C7 C1 123.1(4) . 3_665 ?
O3 C8 O2 123.2(4) . . ?
O3 C8 C9 125.4(4) . . ?
O2 C8 C9 111.4(3) . . ?
C14 C9 C10 118.8(4) . . ?
C14 C9 C8 119.0(4) . . ?
C10 C9 C8 122.3(4) . . ?
C11 C10 C9 119.4(4) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 122.0(4) . . ?
C10 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C11 C12 C13 117.9(4) . . ?
C11 C12 C15 120.1(4) . . ?
C13 C12 C15 122.0(4) . . ?
C14 C13 C12 120.5(4) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C9 121.4(4) . . ?
C13 C14 H14 119.3 . . ?
C9 C14 H14 119.3 . . ?
C16 C15 C19 117.4(4) . . ?
C16 C15 C12 120.6(4) . . ?
C19 C15 C12 121.9(4) . . ?
N1 C16 C15 124.9(4) . . ?
N1 C16 H16 117.5 . . ?
C15 C16 H16 117.5 . . ?
N1 C17 C18 123.3(4) . . ?
N1 C17 H17 118.3 . . ?
C18 C17 H17 118.3 . . ?
C19 C18 C17 118.1(5) . . ?
C19 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
C18 C19 C15 119.6(5) . . ?
C18 C19 H19 120.2 . . ?
C15 C19 H19 120.2 . . ?
O1 C20 H20A 109.5 . . ?
O1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 C22 170(2) . . ?
N3 C23 C24 162(6) . . ?
N4 C25 C26 180.000(4) . . ?
C25 C26 C26 180.000(3) . 7_556 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.04
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.466
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.102