# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Cheng-Yong Su'
_publ_contact_author_email       CESSCY@MAIL.SYSU.EDU.CN

_publ_section_title              
;
Self-assembly of borromean networks
through hydrogen-bonding recognition
;
loop_
_publ_author_name
'Cheng-Yong Su.'
'Ji-Jun Jang.'
'Dai-Bin Kuan.'
'Lei Li.'
'Wei Wang.'
;
Tao Yang
;

# Attachment 'Compds.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 710183'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C102 H84 Cd2 Cl4 N26 O8'
_chemical_formula_weight         2168.55

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'
Cd Cd -0.8075 1.2024 '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                   16.6537(9)
_cell_length_b                   16.6537(9)
_cell_length_c                   33.4873(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     8043.3(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_cell_measurement_reflns_used 2331
_cell_measurement_theta_min      2.7995
_cell_measurement_theta_max      29.7220
_exptl_absorpt_correction_T_min  0.73334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3318
_exptl_absorpt_coefficient_mu    0.562

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measurement_device_type  'Oxford Germini S Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9090
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.81
_diffrn_reflns_theta_max         27.00
_reflns_number_total             3869
_reflns_number_gt                1544
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_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.
;

_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^)+(0.1000P)^2^+14.0000P] 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         3869
_refine_ls_number_parameters     213
_refine_ls_number_restraints     169
_refine_ls_R_factor_all          0.1719
_refine_ls_R_factor_gt           0.0872
_refine_ls_wR_factor_ref         0.2451
_refine_ls_wR_factor_gt          0.2196
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.085
_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
Cd1 Cd 0.0000 0.0000 0.34654(2) 0.1147(6) Uani 1 3 d S . .
Cl1 Cl -0.3333 0.3333 0.45456(7) 0.0663(7) Uani 1 3 d S . .
O1 O -0.2822(5) 0.2952(6) 0.4421(2) 0.172(3) Uani 1 1 d U . .
O2 O -0.3333 0.3333 0.4973(3) 0.168(4) Uani 1 3 d SU . .
N1 N 0.0000 0.0000 0.2688(2) 0.0603(19) Uani 1 3 d SU . .
N2 N -0.0811(3) 0.0654(3) 0.32432(14) 0.0783(15) Uani 1 1 d U . .
N3 N -0.1516(3) 0.1008(3) 0.27639(15) 0.0708(13) Uani 1 1 d U . .
H3A H -0.1714 0.1040 0.2530 0.085 Uiso 1 1 calc R . .
N4 N -0.1003(4) 0.2610(4) 0.13329(17) 0.0839(15) Uani 1 1 d U . .
N5 N 0.0838(4) 0.2901(3) 0.25795(16) 0.0745(14) Uani 1 1 d U . .
C1 C -0.0818(4) 0.0042(4) 0.25605(15) 0.0625(14) Uani 1 1 d U . .
H1A H -0.1343 -0.0581 0.2534 0.075 Uiso 1 1 calc R . .
H1B H -0.0704 0.0345 0.2303 0.075 Uiso 1 1 calc R . .
C2 C -0.1033(4) 0.0577(4) 0.28665(18) 0.0720(16) Uani 1 1 d U . .
C3 C -0.1619(5) 0.1384(4) 0.3113(2) 0.088(2) Uani 1 1 d U . .
C4 C -0.2059(5) 0.1917(5) 0.3180(3) 0.109(2) Uani 1 1 d DU . .
H4A H -0.2331 0.2087 0.2980 0.131 Uiso 1 1 calc R . .
C5 C -0.2038(6) 0.2153(6) 0.3576(3) 0.133(4) Uani 1 1 d DU . .
H5B H -0.2341 0.2476 0.3643 0.159 Uiso 1 1 calc R . .
C6 C -0.1632(7) 0.1967(6) 0.3868(3) 0.130(4) Uani 1 1 d U . .
H6A H -0.1645 0.2173 0.4125 0.155 Uiso 1 1 calc R . .
C7 C -0.1174(6) 0.1457(6) 0.3798(2) 0.124(3) Uani 1 1 d U . .
H7A H -0.0879 0.1326 0.4003 0.149 Uiso 1 1 calc R . .
C8 C -0.1188(5) 0.1160(5) 0.3407(2) 0.090(2) Uani 1 1 d U . .
C9 C -0.0798(5) 0.3232(5) 0.2000(2) 0.102(2) Uani 1 1 d . . .
H9A H -0.0950 0.3536 0.2192 0.122 Uiso 1 1 calc R . .
C10 C -0.1209(6) 0.3048(5) 0.1626(2) 0.105(2) Uani 1 1 d . . .
H10A H -0.1643 0.3229 0.1573 0.125 Uiso 1 1 calc R . .
C11 C -0.0425(5) 0.2301(5) 0.1434(2) 0.090(2) Uani 1 1 d . . .
H11A H -0.0316 0.1948 0.1250 0.108 Uiso 1 1 calc R . .
C12 C 0.0010(5) 0.2484(5) 0.1797(2) 0.0835(19) Uani 1 1 d . . .
H12A H 0.0427 0.2280 0.1848 0.100 Uiso 1 1 calc R . .
C13 C -0.0155(5) 0.2955(4) 0.2082(2) 0.0807(18) Uani 1 1 d . . .
C14 C 0.0298(5) 0.3180(4) 0.2476(2) 0.0846(18) Uani 1 1 d . . .
H14A H 0.0179 0.3539 0.2653 0.102 Uiso 1 1 calc R . .
C15 C 0.1228(4) 0.3130(4) 0.2965(2) 0.0719(17) Uani 1 1 d . . .
C16 C 0.2127(4) 0.3265(4) 0.3008(2) 0.0756(17) Uani 1 1 d . . .
H16A H 0.2429 0.3212 0.2784 0.091 Uiso 1 1 calc R . .
C17 C 0.0770(4) 0.3197(4) 0.33019(10) 0.0730(16) Uani 1 1 d . . .
H17A H 0.0172 0.3102 0.3281 0.088 Uiso 1 1 calc R . .
Cl2 Cl 0.0001(4) 0.0001(4) 0.41801(10) 0.218(3) Uani 1 3 d SRU . .

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
Cd1 0.1498(8) 0.1498(8) 0.0444(5) 0.000 0.000 0.0749(4)
Cl1 0.0682(11) 0.0682(11) 0.0626(14) 0.000 0.000 0.0341(5)
O1 0.180(6) 0.206(7) 0.187(6) -0.056(5) -0.004(5) 0.139(6)
O2 0.209(7) 0.209(7) 0.087(7) 0.000 0.000 0.104(3)
N1 0.068(3) 0.068(3) 0.046(4) 0.000 0.000 0.0338(15)
N2 0.082(3) 0.084(3) 0.051(3) -0.011(2) 0.011(2) 0.029(3)
N3 0.060(3) 0.065(3) 0.078(3) -0.014(2) 0.011(2) 0.024(3)
N4 0.083(4) 0.079(4) 0.096(4) -0.008(3) -0.016(3) 0.045(3)
N5 0.068(3) 0.064(3) 0.090(4) 0.010(3) 0.000(3) 0.032(3)
C1 0.070(3) 0.072(4) 0.050(3) -0.007(2) 0.003(2) 0.039(3)
C2 0.069(4) 0.068(4) 0.069(4) -0.006(3) 0.013(3) 0.027(3)
C3 0.070(4) 0.069(4) 0.105(5) -0.027(4) 0.031(4) 0.021(3)
C4 0.075(4) 0.077(5) 0.150(6) -0.028(4) 0.027(4) 0.019(4)
C5 0.099(6) 0.091(5) 0.161(8) -0.049(6) 0.052(6) 0.012(4)
C6 0.123(7) 0.093(5) 0.115(6) -0.048(5) 0.052(5) 0.010(5)
C7 0.116(6) 0.094(5) 0.086(5) -0.028(4) 0.037(4) -0.004(4)
C8 0.085(4) 0.081(4) 0.068(4) -0.017(3) 0.025(3) 0.014(4)
C9 0.113(6) 0.092(5) 0.117(6) -0.045(4) -0.045(5) 0.064(5)
C10 0.123(6) 0.092(5) 0.118(6) -0.030(4) -0.042(5) 0.069(5)
C11 0.100(5) 0.094(5) 0.087(5) 0.016(4) 0.029(4) 0.057(5)
C12 0.090(5) 0.107(5) 0.076(4) 0.018(4) 0.014(4) 0.066(4)
C13 0.080(5) 0.066(4) 0.103(5) -0.008(3) -0.013(4) 0.042(4)
C14 0.086(5) 0.063(4) 0.105(5) -0.005(3) -0.011(4) 0.037(4)
C15 0.068(4) 0.044(3) 0.097(5) 0.008(3) -0.003(3) 0.023(3)
C16 0.060(4) 0.076(4) 0.095(5) 0.008(3) 0.010(3) 0.038(3)
C17 0.062(4) 0.063(4) 0.096(5) 0.007(3) 0.005(4) 0.032(3)
Cl2 0.302(5) 0.302(5) 0.052(2) 0.000 0.000 0.151(2)

_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
Cd1 N2 2.244(6) 2 ?
Cd1 N2 2.244(6) 3 ?
Cd1 N2 2.244(6) . ?
Cd1 Cl2 2.393(4) . ?
Cd1 N1 2.604(7) . ?
Cl1 O1 1.358(6) . ?
Cl1 O1 1.358(6) 3_455 ?
Cl1 O1 1.358(6) 2_565 ?
Cl1 O2 1.433(11) . ?
N1 C1 1.462(6) 3 ?
N1 C1 1.462(6) . ?
N1 C1 1.462(6) 2 ?
N2 C2 1.303(7) . ?
N2 C8 1.390(9) . ?
N3 C2 1.364(8) . ?
N3 C3 1.375(8) . ?
N3 H3A 0.8600 . ?
N4 C11 1.341(8) . ?
N4 C10 1.365(9) . ?
N5 C14 1.249(7) . ?
N5 C15 1.411(8) . ?
C1 C2 1.514(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 C8 1.375(10) . ?
C3 C4 1.423(10) . ?
C4 C5 1.378(8) . ?
C4 H4A 0.9300 . ?
C5 C6 1.310(14) . ?
C5 H5B 0.9300 . ?
C6 C7 1.417(14) . ?
C6 H6A 0.9300 . ?
C7 C8 1.398(9) . ?
C7 H7A 0.9300 . ?
C9 C10 1.385(10) . ?
C9 C13 1.389(9) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.369(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.348(9) . ?
C12 H12A 0.9300 . ?
C13 C14 1.473(9) . ?
C14 H14A 0.9300 . ?
C15 C17 1.396(8) . ?
C15 C16 1.406(9) . ?
C16 C17 1.352(8) 16 ?
C16 H16A 0.9300 . ?
C17 C16 1.352(8) 16 ?
C17 H17A 0.9300 . ?

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 Cd1 N2 109.57(12) 2 3 ?
N2 Cd1 N2 109.57(12) 2 . ?
N2 Cd1 N2 109.57(12) 3 . ?
N2 Cd1 Cl2 109.41(18) 2 . ?
N2 Cd1 Cl2 109.32(19) 3 . ?
N2 Cd1 Cl2 109.38(19) . . ?
N2 Cd1 N1 70.63(12) 2 . ?
N2 Cd1 N1 70.63(12) 3 . ?
N2 Cd1 N1 70.63(12) . . ?
Cl2 Cd1 N1 179.9(2) . . ?
O1 Cl1 O1 111.0(3) . 3_455 ?
O1 Cl1 O1 111.0(3) . 2_565 ?
O1 Cl1 O1 111.0(3) 3_455 2_565 ?
O1 Cl1 O2 107.9(4) . . ?
O1 Cl1 O2 107.9(4) 3_455 . ?
O1 Cl1 O2 107.9(4) 2_565 . ?
C1 N1 C1 111.9(3) 3 . ?
C1 N1 C1 111.9(3) 3 2 ?
C1 N1 C1 111.9(3) . 2 ?
C1 N1 Cd1 107.0(3) 3 . ?
C1 N1 Cd1 107.0(3) . . ?
C1 N1 Cd1 107.0(3) 2 . ?
C2 N2 C8 104.4(6) . . ?
C2 N2 Cd1 118.9(4) . . ?
C8 N2 Cd1 136.7(5) . . ?
C2 N3 C3 105.4(6) . . ?
C2 N3 H3A 127.3 . . ?
C3 N3 H3A 127.3 . . ?
C11 N4 C10 116.3(6) . . ?
C14 N5 C15 118.1(6) . . ?
N1 C1 C2 109.3(5) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 N3 113.9(5) . . ?
N2 C2 C1 125.0(6) . . ?
N3 C2 C1 121.0(5) . . ?
C8 C3 N3 106.5(6) . . ?
C8 C3 C4 123.8(7) . . ?
N3 C3 C4 129.7(8) . . ?
C5 C4 C3 112.6(9) . . ?
C5 C4 H4A 123.7 . . ?
C3 C4 H4A 123.7 . . ?
C6 C5 C4 126.3(10) . . ?
C6 C5 H5B 116.9 . . ?
C4 C5 H5B 116.9 . . ?
C5 C6 C7 121.0(9) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C8 C7 C6 116.6(10) . . ?
C8 C7 H7A 121.7 . . ?
C6 C7 H7A 121.7 . . ?
C3 C8 N2 109.8(6) . . ?
C3 C8 C7 119.6(8) . . ?
N2 C8 C7 130.6(9) . . ?
C10 C9 C13 118.8(7) . . ?
C10 C9 H9A 120.6 . . ?
C13 C9 H9A 120.6 . . ?
N4 C10 C9 122.7(7) . . ?
N4 C10 H10A 118.6 . . ?
C9 C10 H10A 118.6 . . ?
N4 C11 C12 122.7(6) . . ?
N4 C11 H11A 118.7 . . ?
C12 C11 H11A 118.7 . . ?
C13 C12 C11 121.3(6) . . ?
C13 C12 H12A 119.4 . . ?
C11 C12 H12A 119.4 . . ?
C12 C13 C9 117.9(7) . . ?
C12 C13 C14 123.7(6) . . ?
C9 C13 C14 118.4(6) . . ?
N5 C14 C13 121.7(6) . . ?
N5 C14 H14A 119.1 . . ?
C13 C14 H14A 119.1 . . ?
C17 C15 C16 119.1(6) . . ?
C17 C15 N5 124.4(6) . . ?
C16 C15 N5 116.4(6) . . ?
C17 C16 C15 121.6(6) 16 . ?
C17 C16 H16A 119.2 16 . ?
C15 C16 H16A 119.2 . . ?
C16 C17 C15 119.2(6) 16 . ?
C16 C17 H17A 120.4 16 . ?
C15 C17 H17A 120.4 . . ?

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
N3 H3A N4 0.86 1.99 2.821(8) 163.7 13_455

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.115
#===================#

data_2
_database_code_depnum_ccdc_archive 'CCDC 710184'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C102 H84 Cl4 Mn2 N26 O8'
_chemical_formula_weight         2053.63

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'
Mn Mn 0.3368 0.7283 '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                   16.541(8)
_cell_length_b                   16.541(8)
_cell_length_c                   33.390(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     7912(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1647
_cell_measurement_theta_min      2.7336
_cell_measurement_theta_max      30.1455

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3180
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8875
_exptl_absorpt_correction_T_max  0.9229
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measurement_device_type  'Oxford Germini S Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5974
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.1285
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         25.49
_reflns_number_total             3133
_reflns_number_gt                1071
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_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.
;

_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^)+(0.0810P)^2^+50.0000P] 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     SHELXL
_refine_ls_extinction_coef       0.0116(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3133
_refine_ls_number_parameters     215
_refine_ls_number_restraints     312
_refine_ls_R_factor_all          0.2663
_refine_ls_R_factor_gt           0.1335
_refine_ls_wR_factor_ref         0.3434
_refine_ls_wR_factor_gt          0.3076
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.140
_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
Mn1 Mn 0.3333 -0.3333 0.31960(3) 0.1109(6) Uani 1 3 d SU . .
N1 N 0.3333 -0.3333 0.3986(3) 0.136(3) Uani 1 3 d SU . .
N2 N 0.3994(4) -0.1812(5) 0.34336(19) 0.162(3) Uani 1 1 d U . .
N3 N 0.4337(4) -0.0836(4) 0.3883(2) 0.151(2) Uani 1 1 d U . .
H3A H 0.4368 -0.0601 0.4116 0.182 Uiso 1 1 calc R . .
N4 N 0.2028(4) -0.0851(5) 0.2569(2) 0.155(2) Uani 1 1 d U . .
N5 N 0.3574(4) 0.0976(5) 0.1327(2) 0.163(3) Uani 1 1 d U . .
C1 C 0.3404(5) -0.2433(5) 0.41014(19) 0.128(2) Uani 1 1 d U . .
H1A H 0.2783 -0.2514 0.4124 0.154 Uiso 1 1 calc R . .
H1B H 0.3706 -0.2237 0.4360 0.154 Uiso 1 1 calc R . .
C2 C 0.3923(5) -0.1738(5) 0.3811(2) 0.131(3) Uani 1 1 d U . .
C3 C 0.4716(6) -0.0309(6) 0.3541(3) 0.161(3) Uani 1 1 d U . .
C4 C 0.5260(6) 0.0624(6) 0.3473(3) 0.183(3) Uani 1 1 d U . .
H4 H 0.5440 0.1048 0.3684 0.220 Uiso 1 1 calc R . .
C5 C 0.5538(6) 0.0926(7) 0.3091(3) 0.198(4) Uani 1 1 d U . .
H5A H 0.5878 0.1561 0.3034 0.237 Uiso 1 1 calc R . .
C6 C 0.5305(6) 0.0274(7) 0.2792(3) 0.189(4) Uani 1 1 d U . .
H6A H 0.5518 0.0479 0.2533 0.226 Uiso 1 1 calc R . .
C7 C 0.4763(6) -0.0679(8) 0.2862(3) 0.203(4) Uani 1 1 d U . .
H7A H 0.4573 -0.1115 0.2656 0.244 Uiso 1 1 calc R . .
C8 C 0.4518(6) -0.0944(6) 0.3263(3) 0.164(3) Uani 1 1 d U . .
C9 C 0.4169(6) 0.1087(7) 0.1607(3) 0.188(4) Uani 1 1 d U . .
H9A H 0.4795 0.1473 0.1542 0.225 Uiso 1 1 calc R . .
C10 C 0.2737(6) 0.0442(6) 0.1437(3) 0.167(3) Uani 1 1 d U . .
H10A H 0.2267 0.0351 0.1258 0.200 Uiso 1 1 calc R . .
C11 C 0.2475(6) 0.0000(6) 0.1789(3) 0.171(3) Uani 1 1 d U . .
H11A H 0.1842 -0.0399 0.1836 0.205 Uiso 1 1 calc R . .
C12 C 0.4004(7) 0.0723(7) 0.1973(3) 0.201(4) Uani 1 1 d U . .
H12A H 0.4491 0.0879 0.2152 0.242 Uiso 1 1 calc R . .
C13 C 0.3089(6) 0.0105(6) 0.2083(3) 0.167(3) Uani 1 1 d U . .
C14 C 0.2852(6) -0.0332(6) 0.2471(3) 0.157(3) Uani 1 1 d U . .
H14A H 0.3326 -0.0222 0.2650 0.189 Uiso 1 1 calc R . .
C15 C 0.1885(5) -0.1252(6) 0.2960(3) 0.154(3) Uani 1 1 d U . .
C16 C 0.2412(5) -0.0761(6) 0.3287(3) 0.153(3) Uani 1 1 d U . .
H16A H 0.2914 -0.0159 0.3255 0.184 Uiso 1 1 calc R . .
C17 C 0.1148(6) -0.2155(6) 0.2997(3) 0.163(3) Uani 1 1 d U . .
H17A H 0.0807 -0.2483 0.2773 0.195 Uiso 1 1 calc R . .
Cl1 Cl 0.0000 0.0000 0.12253(9) 0.1296(12) Uani 1 3 d SU . .
O1 O 0.0000 0.0000 0.1649(3) 0.221(5) Uani 1 3 d SU . .
O2 O 0.0464(7) 0.0872(5) 0.1082(3) 0.276(4) Uani 1 1 d U . .
Cl2 Cl 0.3333 -0.3333 0.24771(17) 0.394(5) Uani 1 3 d SU . .

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
Mn1 0.1527(10) 0.1527(10) 0.0274(5) 0.000 0.000 0.0763(5)
N1 0.160(5) 0.160(5) 0.088(5) 0.000 0.000 0.080(2)
N2 0.175(4) 0.199(5) 0.121(4) 0.046(4) 0.015(4) 0.102(3)
N3 0.140(4) 0.171(4) 0.147(4) 0.054(4) 0.020(3) 0.080(3)
N4 0.145(4) 0.158(4) 0.169(5) 0.007(4) 0.019(4) 0.079(3)
N5 0.132(4) 0.168(4) 0.176(5) 0.016(4) -0.002(4) 0.066(3)
C1 0.171(4) 0.122(4) 0.104(4) 0.000(3) 0.015(4) 0.082(3)
C2 0.156(4) 0.138(4) 0.096(4) 0.033(4) 0.027(4) 0.071(4)
C3 0.163(5) 0.172(5) 0.159(5) 0.066(4) 0.015(4) 0.091(4)
C4 0.165(5) 0.198(5) 0.195(6) 0.086(5) 0.029(5) 0.097(4)
C5 0.161(5) 0.226(6) 0.214(7) 0.066(6) 0.023(5) 0.102(5)
C6 0.161(5) 0.213(6) 0.200(6) 0.072(5) 0.013(5) 0.100(5)
C7 0.174(5) 0.244(6) 0.196(6) 0.069(6) 0.011(5) 0.108(5)
C8 0.170(5) 0.197(5) 0.136(5) 0.074(4) 0.026(4) 0.099(4)
C9 0.157(5) 0.221(6) 0.180(6) 0.058(5) 0.001(5) 0.091(5)
C10 0.160(5) 0.174(6) 0.154(6) 0.000(5) 0.013(5) 0.075(4)
C11 0.155(5) 0.183(6) 0.162(6) -0.016(5) 0.015(5) 0.076(4)
C12 0.165(5) 0.215(6) 0.218(7) 0.061(6) 0.001(6) 0.090(5)
C13 0.132(5) 0.187(5) 0.189(6) 0.020(5) 0.000(5) 0.084(4)
C14 0.136(5) 0.164(5) 0.181(6) 0.026(5) 0.013(5) 0.082(4)
C15 0.147(4) 0.148(5) 0.177(5) -0.011(4) 0.014(5) 0.081(4)
C16 0.148(5) 0.146(5) 0.170(6) -0.009(5) -0.002(5) 0.076(4)
C17 0.160(5) 0.149(5) 0.184(7) 0.000(5) 0.018(5) 0.081(4)
Cl1 0.1454(17) 0.1454(17) 0.0981(19) 0.000 0.000 0.0727(8)
O1 0.263(7) 0.263(7) 0.136(7) 0.000 0.000 0.132(3)
O2 0.289(8) 0.143(5) 0.284(7) 0.100(5) 0.043(6) 0.023(5)
Cl2 0.537(8) 0.537(8) 0.108(3) 0.000 0.000 0.269(4)

_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
Mn1 N2 2.325(7) . ?
Mn1 N2 2.325(7) 2_545 ?
Mn1 N2 2.325(7) 3_655 ?
Mn1 Cl2 2.400(6) . ?
Mn1 N1 2.639(9) . ?
N1 C1 1.485(7) . ?
N1 C1 1.485(7) 2_545 ?
N1 C1 1.485(7) 3_655 ?
N2 C2 1.277(9) . ?
N2 C8 1.376(10) . ?
N3 C2 1.317(9) . ?
N3 C3 1.380(10) . ?
N3 H3A 0.8600 . ?
N4 C14 1.239(9) . ?
N4 C15 1.428(11) . ?
N5 C10 1.268(10) . ?
N5 C9 1.304(11) . ?
C1 C2 1.419(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 C8 1.316(12) . ?
C3 C4 1.362(11) . ?
C4 C5 1.363(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(14) . ?
C5 H5A 0.9300 . ?
C6 C7 1.390(13) . ?
C6 H6A 0.9300 . ?
C7 C8 1.403(12) . ?
C7 H7A 0.9300 . ?
C9 C12 1.329(13) . ?
C9 H9A 0.9300 . ?
C10 C11 1.340(11) . ?
C10 H10A 0.9300 . ?
C11 C13 1.359(12) . ?
C11 H11A 0.9300 . ?
C12 C13 1.386(11) . ?
C12 H12A 0.9300 . ?
C13 C14 1.439(12) . ?
C14 H14A 0.9300 . ?
C15 C16 1.381(11) . ?
C15 C17 1.383(10) . ?
C16 C17 1.411(12) 16_545 ?
C16 H16A 0.9300 . ?
C17 C16 1.411(12) 16_545 ?
C17 H17A 0.9300 . ?
Cl1 O2 1.339(7) 2 ?
Cl1 O2 1.339(7) . ?
Cl1 O2 1.339(7) 3 ?
Cl1 O1 1.414(11) . ?

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 Mn1 N2 108.99(16) . 2_545 ?
N2 Mn1 N2 108.99(16) . 3_655 ?
N2 Mn1 N2 108.99(16) 2_545 3_655 ?
N2 Mn1 Cl2 109.95(15) . . ?
N2 Mn1 Cl2 109.95(15) 2_545 . ?
N2 Mn1 Cl2 109.95(15) 3_655 . ?
C1 N1 C1 113.6(3) . 2_545 ?
C1 N1 C1 113.6(3) . 3_655 ?
C1 N1 C1 113.6(3) 2_545 3_655 ?
C2 N2 C8 110.4(7) . . ?
C2 N2 Mn1 115.1(5) . . ?
C8 N2 Mn1 134.3(6) . . ?
C2 N3 C3 112.3(7) . . ?
C2 N3 H3A 123.8 . . ?
C3 N3 H3A 123.8 . . ?
C14 N4 C15 115.7(8) . . ?
C10 N5 C9 112.1(8) . . ?
C2 C1 N1 110.3(6) . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N1 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 N3 105.5(7) . . ?
N2 C2 C1 130.1(7) . . ?
N3 C2 C1 123.7(7) . . ?
C8 C3 C4 123.1(9) . . ?
C8 C3 N3 103.0(8) . . ?
C4 C3 N3 133.5(9) . . ?
C3 C4 C5 118.9(10) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C6 118.8(10) . . ?
C4 C5 H5A 120.6 . . ?
C6 C5 H5A 120.6 . . ?
C5 C6 C7 122.3(10) . . ?
C5 C6 H6A 118.8 . . ?
C7 C6 H6A 118.8 . . ?
C6 C7 C8 116.0(10) . . ?
C6 C7 H7A 122.0 . . ?
C8 C7 H7A 122.0 . . ?
C3 C8 N2 108.5(8) . . ?
C3 C8 C7 120.4(9) . . ?
N2 C8 C7 130.9(9) . . ?
N5 C9 C12 128.8(9) . . ?
N5 C9 H9A 115.6 . . ?
C12 C9 H9A 115.6 . . ?
N5 C10 C11 125.2(10) . . ?
N5 C10 H10A 117.4 . . ?
C11 C10 H10A 117.4 . . ?
C10 C11 C13 123.2(9) . . ?
C10 C11 H11A 118.4 . . ?
C13 C11 H11A 118.4 . . ?
C9 C12 C13 118.6(10) . . ?
C9 C12 H12A 120.7 . . ?
C13 C12 H12A 120.7 . . ?
C11 C13 C12 112.0(9) . . ?
C11 C13 C14 125.9(8) . . ?
C12 C13 C14 122.0(9) . . ?
N4 C14 C13 121.1(9) . . ?
N4 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
C16 C15 C17 121.4(9) . . ?
C16 C15 N4 122.7(7) . . ?
C17 C15 N4 115.8(8) . . ?
C15 C16 C17 119.6(7) . 16_545 ?
C15 C16 H16A 120.2 . . ?
C17 C16 H16A 120.2 16_545 . ?
C15 C17 C16 119.0(8) . 16_545 ?
C15 C17 H17A 120.5 . . ?
C16 C17 H17A 120.5 16_545 . ?
O2 Cl1 O2 107.9(4) 2 . ?
O2 Cl1 O2 107.9(4) 2 3 ?
O2 Cl1 O2 107.9(4) . 3 ?
O2 Cl1 O1 111.0(4) 2 . ?
O2 Cl1 O1 111.0(4) . . ?
O2 Cl1 O1 111.0(4) 3 . ?

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
N3 H3A N5 0.86 2.05 2.888(10) 165.0 6

_diffrn_measured_fraction_theta_max 0.956
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.956
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.073

#================================#

data_3
_database_code_depnum_ccdc_archive 'CCDC 710185'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C102 H98 Cl2 N26 O14'
_chemical_formula_weight         1982.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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                   16.8323(4)
_cell_length_b                   16.8323(4)
_cell_length_c                   32.6236(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     8004.8(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1858
_cell_measurement_theta_min      2.7074
_cell_measurement_theta_max      62.0648
_exptl_absorpt_correction_T_min  0.69571
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3114
_exptl_absorpt_coefficient_mu    1.142

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measurement_device_type  'Oxford Germini S Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5456
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         6.22
_diffrn_reflns_theta_max         60.89
_reflns_number_total             2616
_reflns_number_gt                1543
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_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.

The water molecule encapsulated by ntb (O3) lies on three-fold axis. The other
two solvated water molecules (O4 and O5) are disordered over several positions.
The fractional occupancy (1/3) is assigned to each position, which sums up
two solvated water molecules per ntb ligand.
No H atoms were added for the water molecules due to imposed crystallographic
symmetry or disorder. The ntb compound is protonated with one H^+^ atom
locating on one imino N atom. However, due to 3-fold symmetry of ntb, this H^+^
atom is distributed over three imino N atoms required by the crystallography.
;

_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^)+(0.1000P)^2^+30.0000P] 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         2616
_refine_ls_number_parameters     229
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.1274
_refine_ls_R_factor_gt           0.0959
_refine_ls_wR_factor_ref         0.2571
_refine_ls_wR_factor_gt          0.2424
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

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
N1 N 0.6667 0.3333 0.05110(19) 0.112(2) Uani 1 3 d S . .
N2 N 0.7319(3) 0.2431(3) -0.00207(11) 0.1361(18) Uani 1 1 d . . .
H2A H 0.7121 0.2713 -0.0173 0.163 Uiso 0.33 1 calc PR . .
N3 N 0.7604(2) 0.1812(2) 0.05197(11) 0.1046(12) Uani 1 1 d . . .
H3A H 0.7604 0.1646 0.0769 0.126 Uiso 1 1 calc R . .
N4 N 0.7089(2) -0.0670(2) -0.20159(10) 0.0993(10) Uani 1 1 d . . .
N5 N 0.54971(19) -0.0374(2) -0.07631(10) 0.0922(10) Uani 1 1 d . . .
C1 C 0.6610(3) 0.2479(3) 0.06429(13) 0.1097(15) Uani 1 1 d . . .
H1A H 0.5977 0.1986 0.0632 0.132 Uiso 1 1 calc R . .
H1B H 0.6821 0.2539 0.0924 0.132 Uiso 1 1 calc R . .
C2 C 0.7174(3) 0.2261(3) 0.03775(14) 0.1077(16) Uani 1 1 d . . .
C3 C 0.8042(3) 0.1670(3) 0.01896(15) 0.1193(17) Uani 1 1 d D . .
C4 C 0.8564(3) 0.1249(3) 0.01606(15) 0.1415(19) Uani 1 1 d DU . .
H4A H 0.8678 0.0985 0.0387 0.170 Uiso 1 1 calc R . .
C5 C 0.8911(4) 0.1243(4) -0.02282(17) 0.166(2) Uani 1 1 d DU . .
H5A H 0.9264 0.0966 -0.0270 0.199 Uiso 1 1 calc R . .
C6 C 0.8713(4) 0.1665(4) -0.05543(19) 0.178(3) Uani 1 1 d U . .
H6A H 0.8961 0.1657 -0.0808 0.214 Uiso 1 1 calc R . .
C7 C 0.8198(4) 0.2083(5) -0.05411(18) 0.170(3) Uani 1 1 d U . .
H7A H 0.8085 0.2351 -0.0766 0.204 Uiso 1 1 calc R . .
C8 C 0.7858(4) 0.2059(4) -0.01416(16) 0.145(2) Uani 1 1 d U . .
C9 C 0.7696(3) -0.0267(3) -0.17075(14) 0.1102(15) Uani 1 1 d . . .
H9A H 0.8307 -0.0088 -0.1757 0.132 Uiso 1 1 calc R . .
C10 C 0.7467(3) -0.0106(3) -0.13255(14) 0.1070(15) Uani 1 1 d . . .
H10A H 0.7912 0.0167 -0.1123 0.128 Uiso 1 1 calc R . .
C11 C 0.6218(3) -0.0943(3) -0.19231(14) 0.1070(15) Uani 1 1 d . . .
H11A H 0.5776 -0.1255 -0.2123 0.128 Uiso 1 1 calc R . .
C12 C 0.5929(3) -0.0795(3) -0.15523(14) 0.1044(14) Uani 1 1 d . . .
H12A H 0.5313 -0.0988 -0.1508 0.125 Uiso 1 1 calc R . .
C13 C 0.6567(2) -0.0354(3) -0.12461(13) 0.0913(13) Uani 1 1 d . . .
C14 C 0.6308(2) -0.0163(3) -0.08425(14) 0.0946(13) Uani 1 1 d . . .
H14A H 0.6756 0.0120 -0.0642 0.113 Uiso 1 1 calc R . .
C15 C 0.5283(2) -0.0173(3) -0.03722(13) 0.0882(12) Uani 1 1 d . . .
C16 C 0.4550(2) -0.0011(3) -0.03509(13) 0.0954(13) Uani 1 1 d . . .
H16A H 0.4241 -0.0026 -0.0589 0.115 Uiso 1 1 calc R . .
C17 C 0.5719(2) -0.0170(3) -0.00135(13) 0.0928(13) Uani 1 1 d . . .
H17A H 0.6200 -0.0293 -0.0021 0.111 Uiso 1 1 calc R . .
Cl1 Cl 1.0000 0.0000 0.12240(5) 0.0798(5) Uani 1 3 d S . .
O1 O 0.9146(2) -0.0160(2) 0.11189(15) 0.1643(16) Uani 1 1 d U . .
O2 O 1.0000 0.0000 0.1662(2) 0.184(3) Uani 1 3 d SU . .
O3 O 0.6667 0.3333 -0.0333(3) 0.165(3) Uani 1 3 d SU . .
O4 O 0.7465(12) 0.2092(13) -0.1832(6) 0.239(6) Uani 0.33 1 d PU A -1
O5 O 0.8044(12) 0.3123(13) -0.1703(6) 0.234(6) Uani 0.33 1 d PU B -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 0.124(3) 0.124(3) 0.087(4) 0.000 0.000 0.0618(15)
N2 0.141(3) 0.155(3) 0.081(2) 0.012(2) 0.017(2) 0.051(3)
N3 0.107(2) 0.0887(18) 0.096(2) -0.0175(17) 0.0357(18) 0.0323(16)
N4 0.0949(16) 0.1163(19) 0.098(2) -0.0252(17) -0.0280(17) 0.0615(14)
N5 0.0762(15) 0.1055(18) 0.100(2) 0.0027(17) -0.0044(16) 0.0497(13)
C1 0.121(3) 0.121(3) 0.093(3) 0.008(2) 0.021(2) 0.065(2)
C2 0.114(3) 0.108(3) 0.092(3) -0.002(2) 0.012(2) 0.048(2)
C3 0.106(3) 0.094(3) 0.112(3) -0.034(2) 0.041(2) 0.016(2)
C4 0.111(3) 0.108(3) 0.170(4) -0.050(3) 0.053(3) 0.029(2)
C5 0.118(3) 0.127(3) 0.186(4) -0.069(3) 0.054(3) 0.011(3)
C6 0.120(3) 0.159(4) 0.147(4) -0.071(3) 0.057(3) -0.012(3)
C7 0.140(4) 0.169(4) 0.113(3) -0.044(3) 0.044(3) 0.010(3)
C8 0.125(3) 0.141(4) 0.096(3) -0.031(3) 0.034(3) 0.013(3)
C9 0.085(2) 0.135(3) 0.105(3) -0.042(2) -0.018(2) 0.051(2)
C10 0.079(2) 0.127(3) 0.110(3) -0.046(2) -0.018(2) 0.0484(19)
C11 0.094(2) 0.125(3) 0.106(3) -0.016(2) -0.035(2) 0.057(2)
C12 0.0799(19) 0.134(3) 0.105(3) -0.006(2) -0.021(2) 0.0578(19)
C13 0.0761(19) 0.091(2) 0.105(3) -0.012(2) -0.012(2) 0.0408(16)
C14 0.0727(18) 0.099(2) 0.109(3) -0.008(2) -0.008(2) 0.0410(17)
C15 0.0699(17) 0.091(2) 0.102(3) 0.008(2) -0.0017(19) 0.0393(15)
C16 0.0827(18) 0.122(2) 0.093(3) 0.004(2) -0.008(2) 0.0596(17)
C17 0.0730(17) 0.101(2) 0.112(3) 0.010(2) -0.008(2) 0.0490(16)
Cl1 0.0699(5) 0.0699(5) 0.0996(11) 0.000 0.000 0.0350(3)
O1 0.0955(16) 0.159(2) 0.253(4) -0.036(3) -0.051(2) 0.0744(16)
O2 0.216(4) 0.216(4) 0.121(5) 0.000 0.000 0.108(2)
O3 0.110(2) 0.110(2) 0.275(8) 0.000 0.000 0.0549(12)
O4 0.243(9) 0.258(9) 0.243(10) 0.005(8) 0.010(8) 0.146(7)
O5 0.231(9) 0.250(9) 0.249(10) 0.025(9) 0.005(8) 0.140(7)

_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
N1 C1 1.458(5) . ?
N1 C1 1.458(5) 2_655 ?
N1 C1 1.458(5) 3_665 ?
N2 C2 1.326(6) . ?
N2 C8 1.393(8) . ?
N2 H2A 0.8600 . ?
N3 C2 1.361(6) . ?
N3 C3 1.392(5) . ?
N3 H3A 0.8600 . ?
N4 C11 1.333(5) . ?
N4 C9 1.351(5) . ?
N5 C14 1.254(5) . ?
N5 C15 1.411(5) . ?
C1 C2 1.462(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 C8 1.376(8) . ?
C3 C4 1.379(6) . ?
C4 C5 1.399(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.409(10) . ?
C5 H5A 0.9300 . ?
C6 C7 1.362(11) . ?
C6 H6A 0.9300 . ?
C7 C8 1.416(7) . ?
C7 H7A 0.9300 . ?
C9 C10 1.371(6) . ?
C9 H9A 0.9300 . ?
C10 C13 1.380(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.373(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.380(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.472(6) . ?
C14 H14A 0.9300 . ?
C15 C17 1.380(6) . ?
C15 C16 1.392(6) . ?
C16 C17 1.360(6) 10_655 ?
C16 H16A 0.9300 . ?
C17 C16 1.360(6) 10_655 ?
C17 H17A 0.9300 . ?
Cl1 O1 1.368(3) 2_645 ?
Cl1 O1 1.368(3) . ?
Cl1 O1 1.368(3) 3_765 ?
Cl1 O2 1.427(7) . ?

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
C1 N1 C1 111.7(3) . 2_655 ?
C1 N1 C1 111.7(3) . 3_665 ?
C1 N1 C1 111.7(3) 2_655 3_665 ?
C2 N2 C8 105.7(5) . . ?
C2 N2 H2A 127.2 . . ?
C8 N2 H2A 127.2 . . ?
C2 N3 C3 107.8(4) . . ?
C2 N3 H3A 126.1 . . ?
C3 N3 H3A 126.1 . . ?
C11 N4 C9 115.4(4) . . ?
C14 N5 C15 119.4(3) . . ?
N1 C1 C2 110.1(4) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 N3 111.3(5) . . ?
N2 C2 C1 126.7(5) . . ?
N3 C2 C1 122.0(4) . . ?
C8 C3 C4 122.8(5) . . ?
C8 C3 N3 105.1(5) . . ?
C4 C3 N3 132.1(5) . . ?
C3 C4 C5 116.2(5) . . ?
C3 C4 H4A 121.9 . . ?
C5 C4 H4A 121.9 . . ?
C4 C5 C6 118.4(6) . . ?
C4 C5 H5A 120.8 . . ?
C6 C5 H5A 120.8 . . ?
C7 C6 C5 127.5(6) . . ?
C7 C6 H6A 116.3 . . ?
C5 C6 H6A 116.3 . . ?
C6 C7 C8 111.5(7) . . ?
C6 C7 H7A 124.2 . . ?
C8 C7 H7A 124.2 . . ?
C3 C8 N2 110.1(4) . . ?
C3 C8 C7 123.5(7) . . ?
N2 C8 C7 126.3(7) . . ?
N4 C9 C10 124.0(4) . . ?
N4 C9 H9A 118.0 . . ?
C10 C9 H9A 118.0 . . ?
C9 C10 C13 119.0(4) . . ?
C9 C10 H10A 120.5 . . ?
C13 C10 H10A 120.5 . . ?
N4 C11 C12 124.5(4) . . ?
N4 C11 H11A 117.8 . . ?
C12 C11 H11A 117.8 . . ?
C11 C12 C13 118.9(4) . . ?
C11 C12 H12A 120.5 . . ?
C13 C12 H12A 120.5 . . ?
C12 C13 C10 117.9(4) . . ?
C12 C13 C14 121.9(4) . . ?
C10 C13 C14 120.1(4) . . ?
N5 C14 C13 121.5(4) . . ?
N5 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
C17 C15 C16 118.6(4) . . ?
C17 C15 N5 124.6(4) . . ?
C16 C15 N5 116.7(4) . . ?
C17 C16 C15 121.0(4) 10_655 . ?
C17 C16 H16A 119.5 10_655 . ?
C15 C16 H16A 119.5 . . ?
C16 C17 C15 120.4(4) 10_655 . ?
C16 C17 H17A 119.8 10_655 . ?
C15 C17 H17A 119.8 . . ?
O1 Cl1 O1 113.94(17) 2_645 . ?
O1 Cl1 O1 113.94(17) 2_645 3_765 ?
O1 Cl1 O1 113.94(17) . 3_765 ?
O1 Cl1 O2 104.5(2) 2_645 . ?
O1 Cl1 O2 104.5(2) . . ?
O1 Cl1 O2 104.5(2) 3_765 . ?

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
N2 H2A O3 0.86 1.66 2.494(7) 163.2 .
N3 H3A N4 0.86 1.96 2.811(5) 168.2 5_545

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        60.89
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.066

#==================END