Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2007

data_global

_journal_coden_Cambridge         1350

loop_
_publ_author_name
R.Custelcean
P.V.Bonnesen
N.L.Engle

_publ_contact_author_name        'Radu Custelcean'
_publ_contact_author_address     
;
Chemical Sciences Division
Oak Ridge National Laboratory
PO Box 2008 MS-6119
Oak Ridge
Tennessee
37831-6119
UNITED STATES OF AMERICA
;

_publ_contact_author_email       CUSTELCEANR@ORNL.GOV

_publ_requested_journal          'Cryst Eng. Comm.'

_publ_section_title              
;
Crystalline hydrogen-bonded nanocolumns of cyclic
thiourea octamers
;

data_1
_database_code_depnum_ccdc_archive 'CCDC 635440'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H40 N4 S2'
_chemical_formula_weight         424.70

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   12.586(5)
_cell_length_b                   16.546(7)
_cell_length_c                   26.900(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.338(10)
_cell_angle_gamma                90.00
_cell_volume                     5528(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9353
_exptl_absorpt_correction_T_max  0.9959
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42895
_diffrn_reflns_av_R_equivalents  0.1487
_diffrn_reflns_av_sigmaI/netI    0.1472
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9711
_reflns_number_gt                4399
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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^)+(0.0695P)^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         9711
_refine_ls_number_parameters     517
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.0696
_refine_ls_wR_factor_ref         0.1630
_refine_ls_wR_factor_gt          0.1388
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_restrained_S_all      0.864
_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
S1 S 0.64481(9) 0.88786(7) 0.16462(4) 0.0440(3) Uani 1 1 d . . .
S2 S 0.79881(10) 1.38896(7) 0.00439(4) 0.0470(3) Uani 1 1 d . . .
N3 N 0.8708(3) 1.3803(2) -0.08328(13) 0.0443(10) Uani 1 1 d . . .
H3N H 0.8994 1.3500 -0.1045 0.053 Uiso 1 1 calc R . .
N2 N 0.6499(3) 1.0133(2) 0.10298(12) 0.0415(9) Uani 1 1 d . . .
H2N H 0.6323 1.0633 0.0941 0.050 Uiso 1 1 calc R . .
C5 C 0.6190(3) 0.9838(2) 0.14518(15) 0.0341(10) Uani 1 1 d . . .
C7 C 0.7319(3) 1.0113(2) 0.02455(15) 0.0332(10) Uani 1 1 d . . .
N1 N 0.5644(3) 1.0373(2) 0.16890(13) 0.0549(11) Uani 1 1 d . . .
H1N H 0.5482 1.0827 0.1524 0.066 Uiso 1 1 calc R . .
N4 N 0.8917(3) 1.2654(2) -0.03661(13) 0.0467(10) Uani 1 1 d . . .
H4N H 0.9234 1.2467 -0.0611 0.056 Uiso 1 1 calc R . .
C16 C 0.8189(3) 1.1318(2) -0.01169(15) 0.0318(10) Uani 1 1 d . . .
C19 C 0.8466(3) 1.4645(3) -0.10040(16) 0.0412(11) Uani 1 1 d . . .
C14 C 0.8843(3) 1.0733(3) -0.03823(16) 0.0412(11) Uani 1 1 d . . .
H16A H 0.9533 1.0614 -0.0161 0.049 Uiso 1 1 calc R . .
H16B H 0.9008 1.0986 -0.0694 0.049 Uiso 1 1 calc R . .
C18 C 0.8560(3) 1.3430(2) -0.04063(16) 0.0360(11) Uani 1 1 d . . .
C9 C 0.8224(4) 0.9943(3) -0.05143(17) 0.0450(12) Uani 1 1 d . . .
H20 H 0.8667 0.9570 -0.0690 0.054 Uiso 1 1 calc R . .
C8 C 0.7980(3) 0.9541(3) -0.00350(16) 0.0428(12) Uani 1 1 d . . .
H21A H 0.8663 0.9401 0.0186 0.051 Uiso 1 1 calc R . .
H21B H 0.7572 0.9035 -0.0122 0.051 Uiso 1 1 calc R . .
C15 C 0.7137(3) 1.1500(3) -0.04590(17) 0.0442(12) Uani 1 1 d . . .
H22A H 0.7284 1.1764 -0.0771 0.053 Uiso 1 1 calc R . .
H22B H 0.6701 1.1875 -0.0288 0.053 Uiso 1 1 calc R . .
C13 C 0.7953(3) 1.0904(2) 0.03665(15) 0.0335(10) Uani 1 1 d . . .
H24A H 0.8641 1.0786 0.0590 0.040 Uiso 1 1 calc R . .
H24B H 0.7533 1.1276 0.0548 0.040 Uiso 1 1 calc R . .
C6 C 0.7107(4) 0.9669(3) 0.07135(17) 0.0455(12) Uani 1 1 d . . .
H25A H 0.6708 0.9165 0.0609 0.055 Uiso 1 1 calc R . .
H25B H 0.7806 0.9513 0.0916 0.055 Uiso 1 1 calc R . .
C12 C 0.6268(3) 1.0313(3) -0.01105(17) 0.0483(12) Uani 1 1 d . . .
H28A H 0.5852 0.9810 -0.0197 0.058 Uiso 1 1 calc R . .
H28B H 0.5824 1.0680 0.0061 0.058 Uiso 1 1 calc R . .
C22 C 0.7266(4) 1.4820(3) -0.10729(19) 0.0625(14) Uani 1 1 d . . .
H33A H 0.6877 1.4421 -0.1303 0.094 Uiso 1 1 calc R . .
H33B H 0.7127 1.5363 -0.1214 0.094 Uiso 1 1 calc R . .
H33C H 0.7019 1.4789 -0.0746 0.094 Uiso 1 1 calc R . .
C10 C 0.7177(4) 1.0132(3) -0.08598(17) 0.0571(14) Uani 1 1 d . . .
H36A H 0.6768 0.9627 -0.0948 0.068 Uiso 1 1 calc R . .
H36B H 0.7332 1.0382 -0.1175 0.068 Uiso 1 1 calc R . .
C4 C 0.5266(4) 1.0326(3) 0.21834(16) 0.0495(13) Uani 1 1 d . . .
C17 C 0.8821(4) 1.2106(2) 0.00446(16) 0.0446(12) Uani 1 1 d . . .
H40A H 0.8458 1.2393 0.0293 0.053 Uiso 1 1 calc R . .
H40B H 0.9553 1.1960 0.0215 0.053 Uiso 1 1 calc R . .
C21 C 0.8840(4) 1.4707(3) -0.15116(18) 0.0659(16) Uani 1 1 d . . .
H42A H 0.9622 1.4628 -0.1467 0.099 Uiso 1 1 calc R . .
H42B H 0.8659 1.5243 -0.1657 0.099 Uiso 1 1 calc R . .
H42C H 0.8482 1.4291 -0.1739 0.099 Uiso 1 1 calc R . .
C20 C 0.9093(4) 1.5256(3) -0.06403(19) 0.0665(15) Uani 1 1 d . . .
H43A H 0.8836 1.5233 -0.0315 0.100 Uiso 1 1 calc R . .
H43B H 0.8980 1.5801 -0.0781 0.100 Uiso 1 1 calc R . .
H43C H 0.9862 1.5125 -0.0592 0.100 Uiso 1 1 calc R . .
C11 C 0.6510(4) 1.0713(3) -0.05915(18) 0.0543(13) Uani 1 1 d . . .
H44 H 0.5818 1.0837 -0.0818 0.065 Uiso 1 1 calc R . .
C2 C 0.6211(4) 1.0222(4) 0.25922(18) 0.0732(17) Uani 1 1 d . . .
H47A H 0.6541 0.9693 0.2558 0.110 Uiso 1 1 calc R . .
H47B H 0.5972 1.0257 0.2921 0.110 Uiso 1 1 calc R . .
H47C H 0.6740 1.0648 0.2566 0.110 Uiso 1 1 calc R . .
C1 C 0.4725(7) 1.1144(4) 0.2241(2) 0.138(4) Uani 1 1 d . . .
H48A H 0.5252 1.1579 0.2236 0.207 Uiso 1 1 calc R . .
H48B H 0.4450 1.1157 0.2562 0.207 Uiso 1 1 calc R . .
H48C H 0.4127 1.1220 0.1963 0.207 Uiso 1 1 calc R . .
C3 C 0.4467(4) 0.9649(4) 0.21931(19) 0.086(2) Uani 1 1 d . . .
H49A H 0.3885 0.9703 0.1905 0.129 Uiso 1 1 calc R . .
H49B H 0.4167 0.9675 0.2507 0.129 Uiso 1 1 calc R . .
H49C H 0.4831 0.9129 0.2173 0.129 Uiso 1 1 calc R . .
S3 S 0.07153(9) 0.77680(8) 0.15968(5) 0.0499(3) Uani 1 1 d . . .
S4 S -0.52713(10) 0.78656(8) -0.11306(5) 0.0595(4) Uani 1 1 d . . .
N7 N -0.7066(3) 0.7063(2) -0.10012(13) 0.0427(9) Uani 1 1 d . . .
H7N H -0.7406 0.6821 -0.0781 0.051 Uiso 1 1 calc R . .
N5 N -0.0728(3) 0.8811(2) 0.18711(13) 0.0411(9) Uani 1 1 d . . .
H5N H -0.1415 0.8903 0.1876 0.049 Uiso 1 1 calc R . .
N8 N -0.5740(3) 0.7136(2) -0.03261(13) 0.0428(9) Uani 1 1 d . . .
H8N H -0.6161 0.6829 -0.0175 0.051 Uiso 1 1 calc R . .
C37 C -0.3127(3) 0.7143(2) 0.05975(15) 0.0348(10) Uani 1 1 d . . .
H6A H -0.2681 0.7182 0.0327 0.042 Uiso 1 1 calc R . .
H6B H -0.3203 0.7693 0.0732 0.042 Uiso 1 1 calc R . .
N6 N -0.1412(3) 0.7723(2) 0.14327(13) 0.0429(9) Uani 1 1 d . . .
H6N H -0.2037 0.7962 0.1430 0.052 Uiso 1 1 calc R . .
C38 C -0.4247(3) 0.6813(2) 0.03757(14) 0.0304(10) Uani 1 1 d . . .
C36 C -0.4918(3) 0.6767(2) 0.08014(14) 0.0338(10) Uani 1 1 d . . .
H13A H -0.5645 0.6557 0.0669 0.041 Uiso 1 1 calc R . .
H13B H -0.4998 0.7315 0.0939 0.041 Uiso 1 1 calc R . .
C40 C -0.6075(4) 0.7338(2) -0.08086(16) 0.0367(11) Uani 1 1 d . . .
C26 C 0.0009(4) 0.9443(3) 0.21242(18) 0.0489(13) Uani 1 1 d . . .
C29 C -0.2559(3) 0.6596(2) 0.10205(16) 0.0358(11) Uani 1 1 d . . .
C31 C -0.4364(3) 0.6209(3) 0.12208(16) 0.0407(11) Uani 1 1 d . . .
H26 H -0.4809 0.6186 0.1497 0.049 Uiso 1 1 calc R . .
C39 C -0.4717(3) 0.7400(3) -0.00390(16) 0.0440(12) Uani 1 1 d . . .
H27A H -0.4821 0.7932 0.0115 0.053 Uiso 1 1 calc R . .
H27B H -0.4192 0.7473 -0.0273 0.053 Uiso 1 1 calc R . .
C27 C -0.0531(3) 0.8125(3) 0.16368(15) 0.0374(11) Uani 1 1 d . . .
C30 C -0.3257(3) 0.6548(3) 0.14315(16) 0.0435(12) Uani 1 1 d . . .
H30A H -0.3336 0.7094 0.1572 0.052 Uiso 1 1 calc R . .
H30B H -0.2904 0.6197 0.1708 0.052 Uiso 1 1 calc R . .
C41 C -0.7682(4) 0.7099(3) -0.15217(16) 0.0470(12) Uani 1 1 d . . .
C33 C -0.3577(3) 0.5408(3) 0.0600(2) 0.0502(13) Uani 1 1 d . . .
H32 H -0.3501 0.4853 0.0461 0.060 Uiso 1 1 calc R . .
C28 C -0.1418(3) 0.6910(2) 0.12110(17) 0.0403(11) Uani 1 1 d . . .
H34A H -0.1049 0.6531 0.1467 0.048 Uiso 1 1 calc R . .
H34B H -0.1007 0.6922 0.0927 0.048 Uiso 1 1 calc R . .
C34 C -0.2459(3) 0.5742(3) 0.08049(19) 0.0499(13) Uani 1 1 d . . .
H35A H -0.2020 0.5763 0.0531 0.060 Uiso 1 1 calc R . .
H35B H -0.2093 0.5381 0.1073 0.060 Uiso 1 1 calc R . .
C32 C -0.4263(4) 0.5363(3) 0.1015(2) 0.0564(14) Uani 1 1 d . . .
H37A H -0.4985 0.5146 0.0878 0.068 Uiso 1 1 calc R . .
H37B H -0.3921 0.4999 0.1287 0.068 Uiso 1 1 calc R . .
C35 C -0.4106(3) 0.5958(3) 0.01780(17) 0.0444(12) Uani 1 1 d . . .
H39A H -0.4819 0.5735 0.0031 0.053 Uiso 1 1 calc R . .
H39B H -0.3656 0.5979 -0.0091 0.053 Uiso 1 1 calc R . .
C44 C -0.7969(4) 0.7972(3) -0.16734(19) 0.0679(15) Uani 1 1 d . . .
H41A H -0.8374 0.8214 -0.1429 0.102 Uiso 1 1 calc R . .
H41B H -0.8409 0.7981 -0.2009 0.102 Uiso 1 1 calc R . .
H41C H -0.7307 0.8282 -0.1679 0.102 Uiso 1 1 calc R . .
C24 C -0.0726(4) 1.0077(3) 0.2308(2) 0.0647(15) Uani 1 1 d . . .
H45A H -0.1248 1.0271 0.2023 0.097 Uiso 1 1 calc R . .
H45B H -0.0291 1.0532 0.2460 0.097 Uiso 1 1 calc R . .
H45C H -0.1111 0.9834 0.2560 0.097 Uiso 1 1 calc R . .
C42 C -0.7052(4) 0.6703(3) -0.18936(17) 0.0708(16) Uani 1 1 d . . .
H46A H -0.6407 0.7023 -0.1916 0.106 Uiso 1 1 calc R . .
H46B H -0.7504 0.6675 -0.2226 0.106 Uiso 1 1 calc R . .
H46C H -0.6840 0.6156 -0.1778 0.106 Uiso 1 1 calc R . .
C43 C -0.8716(4) 0.6622(3) -0.14925(19) 0.0677(15) Uani 1 1 d . . .
H50A H -0.8531 0.6068 -0.1383 0.101 Uiso 1 1 calc R . .
H50B H -0.9168 0.6612 -0.1825 0.101 Uiso 1 1 calc R . .
H50C H -0.9110 0.6882 -0.1250 0.101 Uiso 1 1 calc R . .
C23 C 0.0752(4) 0.9100(4) 0.2570(2) 0.0820(19) Uani 1 1 d . . .
H51A H 0.0325 0.8850 0.2802 0.123 Uiso 1 1 calc R . .
H51B H 0.1194 0.9534 0.2743 0.123 Uiso 1 1 calc R . .
H51C H 0.1220 0.8691 0.2453 0.123 Uiso 1 1 calc R . .
C25 C 0.0633(5) 0.9837(3) 0.1753(2) 0.094(2) Uani 1 1 d . . .
H53A H 0.1137 0.9444 0.1649 0.140 Uiso 1 1 calc R . .
H53B H 0.1035 1.0301 0.1913 0.140 Uiso 1 1 calc R . .
H53C H 0.0131 1.0019 0.1457 0.140 Uiso 1 1 calc R . .

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
S1 0.0542(8) 0.0391(6) 0.0419(7) 0.0031(6) 0.0175(6) 0.0046(6)
S2 0.0629(8) 0.0429(7) 0.0396(7) -0.0028(6) 0.0214(6) -0.0043(6)
N3 0.057(2) 0.036(2) 0.047(2) 0.0051(18) 0.028(2) 0.0082(18)
N2 0.058(2) 0.034(2) 0.039(2) 0.0066(17) 0.026(2) 0.0063(18)
C5 0.033(2) 0.037(2) 0.034(2) -0.006(2) 0.010(2) 0.002(2)
C7 0.031(3) 0.041(3) 0.031(2) 0.002(2) 0.012(2) -0.007(2)
N1 0.085(3) 0.052(2) 0.036(2) 0.0166(19) 0.035(2) 0.030(2)
N4 0.062(3) 0.036(2) 0.049(2) 0.0035(18) 0.029(2) 0.0033(19)
C16 0.027(2) 0.036(3) 0.033(2) 0.0031(19) 0.009(2) 0.0011(19)
C19 0.045(3) 0.043(3) 0.039(3) 0.006(2) 0.016(2) 0.003(2)
C14 0.038(3) 0.050(3) 0.039(3) 0.008(2) 0.018(2) -0.001(2)
C18 0.036(3) 0.034(3) 0.040(3) 0.006(2) 0.011(2) -0.009(2)
C9 0.048(3) 0.047(3) 0.046(3) -0.014(2) 0.026(3) -0.002(2)
C8 0.041(3) 0.044(3) 0.048(3) -0.011(2) 0.021(2) -0.006(2)
C15 0.036(3) 0.057(3) 0.039(3) 0.014(2) 0.007(2) 0.008(2)
C13 0.034(2) 0.035(2) 0.032(2) -0.0022(19) 0.005(2) 0.0064(19)
C6 0.051(3) 0.040(3) 0.052(3) -0.007(2) 0.027(3) 0.000(2)
C12 0.030(3) 0.057(3) 0.060(3) -0.005(3) 0.012(3) -0.010(2)
C22 0.055(3) 0.077(4) 0.053(3) 0.016(3) 0.003(3) 0.007(3)
C10 0.063(4) 0.071(4) 0.039(3) -0.011(3) 0.012(3) -0.024(3)
C4 0.066(3) 0.057(3) 0.031(3) 0.011(2) 0.024(3) 0.021(3)
C17 0.054(3) 0.038(3) 0.042(3) 0.009(2) 0.010(2) 0.000(2)
C21 0.084(4) 0.065(3) 0.058(3) 0.021(3) 0.040(3) 0.012(3)
C20 0.081(4) 0.056(3) 0.060(3) 0.009(3) 0.006(3) -0.019(3)
C11 0.031(3) 0.085(4) 0.044(3) 0.007(3) -0.003(2) -0.006(3)
C2 0.074(4) 0.109(5) 0.037(3) -0.016(3) 0.009(3) 0.006(3)
C1 0.243(9) 0.113(6) 0.089(5) 0.048(4) 0.118(6) 0.104(6)
C3 0.061(4) 0.154(6) 0.052(4) -0.023(4) 0.034(3) -0.026(4)
S3 0.0346(7) 0.0628(8) 0.0534(8) -0.0186(6) 0.0101(6) -0.0029(6)
S4 0.0572(8) 0.0690(9) 0.0536(8) 0.0278(7) 0.0124(7) 0.0034(7)
N7 0.047(2) 0.049(2) 0.032(2) 0.0046(18) 0.006(2) 0.001(2)
N5 0.032(2) 0.042(2) 0.049(2) -0.0185(19) 0.0069(19) -0.0030(18)
N8 0.043(2) 0.057(2) 0.028(2) 0.0121(18) 0.0041(19) -0.0079(19)
C37 0.035(3) 0.038(2) 0.030(2) -0.008(2) 0.002(2) -0.001(2)
N6 0.033(2) 0.036(2) 0.056(3) -0.0171(19) -0.003(2) 0.0007(18)
C38 0.026(2) 0.035(2) 0.028(2) -0.0039(19) -0.003(2) -0.0010(19)
C36 0.028(2) 0.037(2) 0.035(3) -0.002(2) 0.000(2) 0.002(2)
C40 0.044(3) 0.033(3) 0.033(3) 0.002(2) 0.004(2) 0.013(2)
C26 0.054(3) 0.049(3) 0.046(3) -0.015(2) 0.014(3) -0.017(3)
C29 0.026(2) 0.036(2) 0.043(3) -0.010(2) -0.002(2) 0.004(2)
C31 0.037(3) 0.045(3) 0.039(3) 0.010(2) 0.002(2) 0.003(2)
C39 0.037(3) 0.053(3) 0.039(3) 0.005(2) -0.002(2) -0.005(2)
C27 0.045(3) 0.040(3) 0.026(2) 0.001(2) 0.004(2) -0.002(2)
C30 0.043(3) 0.044(3) 0.039(3) 0.007(2) -0.008(2) 0.005(2)
C41 0.056(3) 0.049(3) 0.030(3) 0.001(2) -0.008(2) 0.008(3)
C33 0.033(3) 0.030(3) 0.081(4) -0.022(3) -0.009(3) 0.006(2)
C28 0.033(3) 0.038(3) 0.047(3) -0.011(2) -0.004(2) 0.007(2)
C34 0.036(3) 0.037(3) 0.072(4) -0.013(2) -0.005(3) 0.010(2)
C32 0.043(3) 0.038(3) 0.081(4) 0.016(3) -0.009(3) -0.003(2)
C35 0.032(3) 0.053(3) 0.048(3) -0.018(2) 0.004(2) -0.007(2)
C44 0.087(4) 0.056(3) 0.051(3) -0.005(3) -0.017(3) 0.014(3)
C24 0.072(4) 0.054(3) 0.070(4) -0.029(3) 0.018(3) -0.013(3)
C42 0.100(4) 0.076(4) 0.036(3) -0.010(3) 0.008(3) 0.020(3)
C43 0.067(4) 0.083(4) 0.045(3) -0.003(3) -0.016(3) -0.009(3)
C23 0.072(4) 0.100(5) 0.066(4) -0.033(4) -0.014(3) 0.000(3)
C25 0.126(5) 0.072(4) 0.099(5) -0.034(4) 0.068(4) -0.052(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
S1 C5 1.687(4) . ?
S2 C18 1.687(4) . ?
N3 C18 1.342(5) . ?
N3 C19 1.482(5) . ?
N2 C5 1.349(5) . ?
N2 C6 1.453(5) . ?
C5 N1 1.344(5) . ?
C7 C6 1.519(5) . ?
C7 C8 1.537(5) . ?
C7 C12 1.538(6) . ?
C7 C13 1.540(5) . ?
N1 C4 1.485(5) . ?
N4 C18 1.359(5) . ?
N4 C17 1.449(5) . ?
C16 C15 1.516(6) . ?
C16 C14 1.521(5) . ?
C16 C13 1.540(5) . ?
C16 C17 1.553(6) . ?
C19 C21 1.519(6) . ?
C19 C22 1.519(6) . ?
C19 C20 1.534(6) . ?
C14 C9 1.534(6) . ?
C9 C10 1.516(6) . ?
C9 C8 1.525(6) . ?
C15 C11 1.534(6) . ?
C12 C11 1.528(6) . ?
C10 C11 1.532(6) . ?
C4 C2 1.493(7) . ?
C4 C3 1.509(7) . ?
C4 C1 1.535(7) . ?
S3 C27 1.695(4) . ?
S4 C40 1.679(4) . ?
N7 C40 1.350(5) . ?
N7 C41 1.487(5) . ?
N5 C27 1.341(5) . ?
N5 C26 1.489(5) . ?
N8 C40 1.340(5) . ?
N8 C39 1.457(5) . ?
C37 C29 1.536(6) . ?
C37 C38 1.539(5) . ?
N6 C27 1.332(5) . ?
N6 C28 1.470(5) . ?
C38 C39 1.524(6) . ?
C38 C36 1.531(5) . ?
C38 C35 1.532(5) . ?
C36 C31 1.535(5) . ?
C26 C23 1.506(7) . ?
C26 C25 1.513(6) . ?
C26 C24 1.534(6) . ?
C29 C30 1.522(6) . ?
C29 C28 1.535(5) . ?
C29 C34 1.541(5) . ?
C31 C32 1.519(6) . ?
C31 C30 1.524(6) . ?
C41 C42 1.522(6) . ?
C41 C44 1.530(6) . ?
C41 C43 1.534(6) . ?
C33 C32 1.520(6) . ?
C33 C35 1.521(6) . ?
C33 C34 1.529(6) . ?

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
C18 N3 C19 130.4(3) . . ?
C5 N2 C6 123.5(3) . . ?
N1 C5 N2 113.7(4) . . ?
N1 C5 S1 124.1(3) . . ?
N2 C5 S1 122.3(3) . . ?
C6 C7 C8 106.9(3) . . ?
C6 C7 C12 111.8(3) . . ?
C8 C7 C12 107.8(3) . . ?
C6 C7 C13 113.0(3) . . ?
C8 C7 C13 108.9(3) . . ?
C12 C7 C13 108.3(3) . . ?
C5 N1 C4 130.8(4) . . ?
C18 N4 C17 125.7(3) . . ?
C15 C16 C14 109.1(3) . . ?
C15 C16 C13 109.4(3) . . ?
C14 C16 C13 107.9(3) . . ?
C15 C16 C17 111.1(3) . . ?
C14 C16 C17 112.0(3) . . ?
C13 C16 C17 107.3(3) . . ?
N3 C19 C21 105.4(3) . . ?
N3 C19 C22 111.6(4) . . ?
C21 C19 C22 108.9(4) . . ?
N3 C19 C20 111.3(4) . . ?
C21 C19 C20 109.0(4) . . ?
C22 C19 C20 110.5(4) . . ?
C16 C14 C9 111.0(3) . . ?
N3 C18 N4 114.4(4) . . ?
N3 C18 S2 122.7(3) . . ?
N4 C18 S2 122.9(3) . . ?
C10 C9 C8 109.5(4) . . ?
C10 C9 C14 108.9(4) . . ?
C8 C9 C14 109.9(4) . . ?
C9 C8 C7 110.2(4) . . ?
C16 C15 C11 109.7(4) . . ?
C7 C13 C16 111.3(3) . . ?
N2 C6 C7 114.2(3) . . ?
C11 C12 C7 110.5(3) . . ?
C9 C10 C11 109.2(4) . . ?
N1 C4 C2 109.5(4) . . ?
N1 C4 C3 111.4(4) . . ?
C2 C4 C3 110.8(4) . . ?
N1 C4 C1 104.9(4) . . ?
C2 C4 C1 109.9(5) . . ?
C3 C4 C1 110.2(5) . . ?
N4 C17 C16 114.5(4) . . ?
C12 C11 C10 109.1(4) . . ?
C12 C11 C15 109.7(4) . . ?
C10 C11 C15 110.0(4) . . ?
C40 N7 C41 131.0(4) . . ?
C27 N5 C26 131.3(4) . . ?
C40 N8 C39 123.4(4) . . ?
C29 C37 C38 111.5(3) . . ?
C27 N6 C28 125.0(3) . . ?
C39 C38 C36 112.5(3) . . ?
C39 C38 C35 112.8(3) . . ?
C36 C38 C35 108.8(3) . . ?
C39 C38 C37 106.3(3) . . ?
C36 C38 C37 108.0(3) . . ?
C35 C38 C37 108.2(3) . . ?
C38 C36 C31 109.9(3) . . ?
N8 C40 N7 114.4(4) . . ?
N8 C40 S4 120.5(4) . . ?
N7 C40 S4 125.0(3) . . ?
N5 C26 C23 111.0(4) . . ?
N5 C26 C25 110.6(4) . . ?
C23 C26 C25 111.5(5) . . ?
N5 C26 C24 105.3(4) . . ?
C23 C26 C24 109.3(4) . . ?
C25 C26 C24 108.9(4) . . ?
C30 C29 C28 113.2(3) . . ?
C30 C29 C37 108.3(3) . . ?
C28 C29 C37 110.3(3) . . ?
C30 C29 C34 108.5(4) . . ?
C28 C29 C34 107.9(3) . . ?
C37 C29 C34 108.5(3) . . ?
C32 C31 C30 110.4(3) . . ?
C32 C31 C36 110.0(4) . . ?
C30 C31 C36 109.3(3) . . ?
N8 C39 C38 113.7(3) . . ?
N6 C27 N5 114.3(4) . . ?
N6 C27 S3 121.1(3) . . ?
N5 C27 S3 124.6(3) . . ?
C29 C30 C31 110.5(3) . . ?
N7 C41 C42 110.7(4) . . ?
N7 C41 C44 110.7(4) . . ?
C42 C41 C44 110.9(4) . . ?
N7 C41 C43 104.4(4) . . ?
C42 C41 C43 110.5(4) . . ?
C44 C41 C43 109.5(4) . . ?
C32 C33 C35 110.2(3) . . ?
C32 C33 C34 110.6(4) . . ?
C35 C33 C34 108.6(4) . . ?
N6 C28 C29 112.8(3) . . ?
C33 C34 C29 110.0(3) . . ?
C31 C32 C33 108.3(4) . . ?
C33 C35 C38 110.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.055