Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2005

data_global

_journal_coden_Cambridge         222

_publ_requested_journal          'J.C.S. Dalton Transactions'

_publ_contact_author_name        'Dr Stephen Faulkner'

_publ_contact_author_address     
;
School of Chemistry
University of Manchester
Oxford Road
Manchester
M13 9PL
UNITED KINGDOM
;
_publ_contact_author_email       stephen.faulkner@manchester.ac.uk
_publ_contact_author_phone       ?
loop_
_publ_author_name
'Benjamin J. Coe'
'Stephen Faulkner'
'Simon J. A. Pope'
'Rebecca H. Laye'

_publ_section_title              
;
Metal-to-ligand charge-transfer sensitisation of
near-infrared emitting lanthanides in trimetallic arrays M2Ln (M = Ru,
Re or Os; Ln = Nd, Er or Yb)
;

data_9H((CH3)2CO(0.8H2O
_database_code_depnum_ccdc_archive 'CCDC 263036'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_publ_section_exptl_refinement   
;
The structure was solved by direct methods.
The crystal was extremly temperature dependent
and the data was cut at 0.9 angstroms.The remaining
electron density surrounds a disordered PO4H2 molecule
and disordered acetone molecule. Hydrogens were not
included on any of the disordered PO4H2 molecules,
the disordered acetone molecule or the water molecule.
Hydrogens on the ruthenium complex were included
in calculated positions using the riding model.
The unit cell contents and atom list do not match
because not all the positions of the hydrogens have been
calculated but they have been included in the unit cell list.
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H46.60 N8 O14.80 P3 Ru'
_chemical_formula_weight         1034.20

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.7974(14)
_cell_length_b                   12.1158(16)
_cell_length_c                   17.545(2)
_cell_angle_alpha                106.729(2)
_cell_angle_beta                 95.920(2)
_cell_angle_gamma                91.912(2)
_cell_volume                     2181.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9661
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      22.78

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8317
_exptl_absorpt_correction_T_max  0.9732
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      373(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  'CCD area'
_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            9633
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         23.25
_reflns_number_total             6167
_reflns_number_gt                4716
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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^)+(0.1570P)^2^+9.6025P] 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         6167
_refine_ls_number_parameters     558
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0829
_refine_ls_wR_factor_ref         0.2560
_refine_ls_wR_factor_gt          0.2346
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.065
_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
Ru1 Ru 0.11213(7) 0.28785(6) 0.21209(4) 0.0364(3) Uani 1 1 d . . .
N1 N 0.0982(7) 0.4136(6) 0.3179(4) 0.0366(17) Uani 1 1 d . . .
N2 N 0.2645(7) 0.2629(5) 0.2829(4) 0.0346(17) Uani 1 1 d . . .
N3 N 0.5783(7) 0.2745(6) 0.5258(4) 0.0411(18) Uani 1 1 d . . .
H3N H 0.5377 0.3358 0.5383 0.049 Uiso 1 1 calc R . .
N4 N 0.5361(8) 0.1038(7) 0.6149(5) 0.049(2) Uani 1 1 d . . .
H4A H 0.5031 0.0838 0.6539 0.074 Uiso 1 1 calc R . .
H4B H 0.5863 0.0502 0.5922 0.074 Uiso 1 1 calc R . .
H4C H 0.4754 0.1098 0.5783 0.074 Uiso 1 1 calc R . .
O1 O 0.6138(6) 0.1157(5) 0.4274(4) 0.0446(15) Uani 1 1 d . . .
C1 C 0.1879(8) 0.4202(7) 0.3788(5) 0.0321(19) Uani 1 1 d . . .
C2 C 0.0115(9) 0.4922(8) 0.3316(6) 0.043(2) Uani 1 1 d . . .
H2 H -0.0501 0.4898 0.2899 0.051 Uiso 1 1 calc R . .
C3 C 0.0087(9) 0.5766(8) 0.4042(5) 0.043(2) Uani 1 1 d . . .
H3 H -0.0552 0.6270 0.4111 0.051 Uiso 1 1 calc R . .
C4 C 0.1019(8) 0.5847(7) 0.4656(5) 0.039(2) Uani 1 1 d . . .
C5 C 0.1925(8) 0.5038(7) 0.4527(5) 0.0323(19) Uani 1 1 d . . .
H5 H 0.2557 0.5058 0.4934 0.039 Uiso 1 1 calc R . .
C6 C 0.2810(8) 0.3316(7) 0.3599(5) 0.0333(19) Uani 1 1 d . . .
C7 C 0.3479(8) 0.1793(7) 0.2621(5) 0.036(2) Uani 1 1 d . . .
H7 H 0.3404 0.1321 0.2095 0.043 Uiso 1 1 calc R . .
C8 C 0.4405(9) 0.1628(7) 0.3148(5) 0.036(2) Uani 1 1 d . . .
H8 H 0.4943 0.1046 0.2979 0.043 Uiso 1 1 calc R . .
C9 C 0.4564(8) 0.2316(7) 0.3940(5) 0.0341(19) Uani 1 1 d . . .
C10 C 0.3750(8) 0.3184(7) 0.4165(5) 0.0308(18) Uani 1 1 d . . .
H10 H 0.3832 0.3671 0.4688 0.037 Uiso 1 1 calc R . .
C11 C 0.1061(9) 0.6779(8) 0.5435(6) 0.047(2) Uani 1 1 d . . .
H11A H 0.0242 0.6839 0.5604 0.070 Uiso 1 1 calc R . .
H11B H 0.1342 0.7501 0.5367 0.070 Uiso 1 1 calc R . .
H11C H 0.1626 0.6595 0.5834 0.070 Uiso 1 1 calc R . .
C12 C 0.5561(8) 0.2030(7) 0.4511(5) 0.035(2) Uani 1 1 d . . .
C13 C 0.6669(9) 0.2529(8) 0.5856(5) 0.044(2) Uani 1 1 d . . .
H13A H 0.7193 0.3230 0.6117 0.053 Uiso 1 1 calc R . .
H13B H 0.7202 0.1941 0.5596 0.053 Uiso 1 1 calc R . .
C14 C 0.6072(10) 0.2139(8) 0.6482(6) 0.050(2) Uani 1 1 d . . .
H14A H 0.6718 0.2075 0.6892 0.060 Uiso 1 1 calc R . .
H14B H 0.5524 0.2717 0.6735 0.060 Uiso 1 1 calc R . .
N5 N -0.0073(7) 0.1811(6) 0.2466(4) 0.0419(18) Uani 1 1 d . . .
N6 N -0.0557(8) 0.3132(7) 0.1552(4) 0.048(2) Uani 1 1 d . . .
C15 C -0.1305(9) 0.1859(8) 0.2237(6) 0.050(3) Uani 1 1 d . . .
C16 C 0.0252(11) 0.1112(8) 0.2916(6) 0.053(3) Uani 1 1 d . . .
H16 H 0.1094 0.1067 0.3074 0.064 Uiso 1 1 calc R . .
C17 C -0.0633(11) 0.0450(9) 0.3152(6) 0.057(3) Uani 1 1 d . . .
H17 H -0.0382 -0.0029 0.3460 0.069 Uiso 1 1 calc R . .
C18 C -0.1853(12) 0.0512(9) 0.2928(7) 0.063(3) Uani 1 1 d . . .
H18 H -0.2449 0.0081 0.3088 0.076 Uiso 1 1 calc R . .
C19 C -0.2220(10) 0.1207(9) 0.2468(6) 0.059(3) Uani 1 1 d . . .
H19 H -0.3062 0.1249 0.2309 0.071 Uiso 1 1 calc R . .
C20 C -0.1589(9) 0.2593(8) 0.1722(6) 0.049(2) Uani 1 1 d . . .
C21 C -0.0735(12) 0.3811(11) 0.1053(6) 0.067(3) Uani 1 1 d . . .
H21 H -0.0040 0.4182 0.0939 0.080 Uiso 1 1 calc R . .
C22 C -0.1888(11) 0.3972(12) 0.0712(8) 0.075(4) Uani 1 1 d . . .
H22 H -0.1963 0.4415 0.0357 0.090 Uiso 1 1 calc R . .
C23 C -0.2921(13) 0.3478(14) 0.0896(8) 0.088(4) Uani 1 1 d . . .
H23 H -0.3715 0.3617 0.0699 0.105 Uiso 1 1 calc R . .
C24 C -0.2762(10) 0.2743(11) 0.1399(7) 0.066(3) Uani 1 1 d . . .
H24 H -0.3454 0.2364 0.1509 0.080 Uiso 1 1 calc R . .
N7 N 0.1572(7) 0.1674(6) 0.1115(4) 0.0436(19) Uani 1 1 d . . .
N8 N 0.2190(7) 0.3891(6) 0.1643(4) 0.0388(17) Uani 1 1 d . . .
C25 C 0.2395(10) 0.2070(8) 0.0692(5) 0.046(2) Uani 1 1 d . . .
C26 C 0.1233(10) 0.0530(8) 0.0876(5) 0.048(2) Uani 1 1 d . . .
H26 H 0.0662 0.0247 0.1148 0.058 Uiso 1 1 calc R . .
C27 C 0.1701(12) -0.0222(9) 0.0248(6) 0.064(3) Uani 1 1 d . . .
H27 H 0.1432 -0.1000 0.0095 0.077 Uiso 1 1 calc R . .
C28 C 0.2556(15) 0.0151(9) -0.0156(7) 0.084(4) Uani 1 1 d . . .
H28 H 0.2904 -0.0364 -0.0567 0.101 Uiso 1 1 calc R . .
C29 C 0.2893(13) 0.1331(9) 0.0066(6) 0.067(3) Uani 1 1 d . . .
H29 H 0.3455 0.1617 -0.0209 0.081 Uiso 1 1 calc R . .
C30 C 0.2705(9) 0.3320(8) 0.0971(5) 0.042(2) Uani 1 1 d . . .
C31 C 0.2399(10) 0.5046(8) 0.1915(5) 0.047(2) Uani 1 1 d . . .
H31 H 0.2041 0.5447 0.2366 0.056 Uiso 1 1 calc R . .
C32 C 0.3121(10) 0.5662(8) 0.1554(6) 0.049(2) Uani 1 1 d . . .
H32 H 0.3246 0.6461 0.1760 0.059 Uiso 1 1 calc R . .
C33 C 0.3656(10) 0.5081(8) 0.0885(6) 0.050(2) Uani 1 1 d . . .
H33 H 0.4149 0.5480 0.0634 0.060 Uiso 1 1 calc R . .
C34 C 0.3450(9) 0.3908(8) 0.0596(5) 0.046(2) Uani 1 1 d . . .
H34 H 0.3809 0.3503 0.0147 0.055 Uiso 1 1 calc R . .
P1 P 0.3986(3) 0.5130(3) 0.67878(17) 0.0646(9) Uani 1 1 d . . .
O2' O 0.5057(16) 0.5782(15) 0.7411(9) 0.031(5) Uiso 0.416(16) 1 d P A 1
O3' O 0.4680(19) 0.4698(15) 0.6051(10) 0.034(5) Uiso 0.416(16) 1 d P A 1
O4' O 0.2803(17) 0.5458(15) 0.6740(10) 0.058(6) Uiso 0.416(16) 1 d P A 1
O5' O 0.4085(19) 0.4173(18) 0.7251(12) 0.076(7) Uiso 0.416(16) 1 d P A 1
O2" O 0.4824(14) 0.6086(14) 0.7399(9) 0.053(5) Uiso 0.584(16) 1 d P A 2
O3" O 0.4282(16) 0.4705(13) 0.6003(9) 0.052(5) Uiso 0.584(16) 1 d P A 2
O4" O 0.3326(10) 0.6364(10) 0.6722(7) 0.049(4) Uiso 0.584(16) 1 d P A 2
O5" O 0.3000(15) 0.4727(14) 0.7159(10) 0.088(6) Uiso 0.584(16) 1 d P A 2
P2 P 0.5205(4) 0.1351(3) 0.8476(2) 0.0858(12) Uani 1 1 d . . .
O6' O 0.4877(15) 0.0222(13) 0.8712(9) 0.054(5) Uiso 0.64(2) 1 d P B 1
O7' O 0.4389(15) 0.1210(12) 0.7633(8) 0.056(4) Uiso 0.64(2) 1 d P B 1
O8' O 0.6607(12) 0.1205(11) 0.8327(9) 0.058(4) Uiso 0.64(2) 1 d P B 1
O9' O 0.5048(11) 0.2342(9) 0.9103(7) 0.055(4) Uiso 0.64(2) 1 d P B 1
O6" O 0.522(2) 0.0197(17) 0.8801(12) 0.030(6) Uiso 0.36(2) 1 d P B 2
O7" O 0.477(2) 0.0957(17) 0.7655(11) 0.034(5) Uiso 0.36(2) 1 d P B 2
O8" O 0.671(3) 0.109(3) 0.863(2) 0.097(11) Uiso 0.36(2) 1 d P B 2
O9" O 0.419(2) 0.2475(19) 0.8739(13) 0.067(8) Uiso 0.36(2) 1 d P B 2
P3 P 0.2169(4) 0.0958(4) 0.5100(3) 0.0852(11) Uani 1 1 d . . .
O10' O 0.241(3) 0.027(3) 0.421(2) 0.126(13) Uiso 0.368(17) 1 d P C 1
O11' O 0.123(2) 0.157(2) 0.4712(14) 0.055(7) Uiso 0.368(17) 1 d P C 1
O12' O 0.131(2) 0.013(2) 0.5215(19) 0.078(8) Uiso 0.368(17) 1 d P C 1
O13' O 0.307(4) 0.152(3) 0.582(2) 0.131(13) Uiso 0.368(17) 1 d P C 1
O10" O 0.3397(9) 0.0777(8) 0.4843(6) 0.042(3) Uiso 0.632(17) 1 d P C 2
O11" O 0.1521(15) 0.1934(15) 0.4833(10) 0.069(5) Uiso 0.632(17) 1 d P C 2
O12" O 0.1313(13) -0.0146(13) 0.4798(10) 0.073(4) Uiso 0.632(17) 1 d P C 2
O13" O 0.2165(15) 0.1398(13) 0.6042(9) 0.086(5) Uiso 0.632(17) 1 d P C 2
O1S O -0.011(2) 0.6250(15) 0.0673(10) 0.266(12) Uani 1 1 d D D .
C1S C -0.0055(15) 0.7222(13) 0.1288(10) 0.092(4) Uiso 1 1 d D . .
C2S' C -0.078(5) 0.826(3) 0.140(3) 0.06(2) Uiso 0.25(6) 1 d PD D 1
C2S" C -0.025(5) 0.8365(18) 0.113(2) 0.190(17) Uiso 0.75(6) 1 d PD D 2
C3S' C 0.079(10) 0.754(7) 0.206(4) 0.17(5) Uiso 0.25(6) 1 d PD D 1
C3S" C 0.001(5) 0.714(3) 0.2145(12) 0.22(2) Uiso 0.75(6) 1 d PD D 2
O2S O 0.2642(12) 0.2646(11) 0.7423(8) 0.100(4) Uiso 0.80 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ru1 0.0434(5) 0.0338(4) 0.0280(4) 0.0040(3) 0.0031(3) -0.0056(3)
N1 0.043(4) 0.034(4) 0.032(4) 0.006(3) 0.010(3) 0.000(3)
N2 0.047(4) 0.024(3) 0.031(4) 0.005(3) 0.008(3) -0.012(3)
N3 0.055(5) 0.038(4) 0.030(4) 0.011(3) 0.002(3) -0.006(4)
N4 0.059(5) 0.048(5) 0.042(5) 0.019(4) 0.002(4) -0.006(4)
O1 0.049(4) 0.038(4) 0.045(4) 0.009(3) 0.004(3) 0.006(3)
C1 0.045(5) 0.025(4) 0.028(4) 0.009(3) 0.011(4) -0.004(4)
C2 0.042(5) 0.040(5) 0.042(5) 0.007(4) 0.001(4) 0.000(4)
C3 0.041(5) 0.045(5) 0.038(5) 0.004(4) 0.009(4) 0.002(4)
C4 0.045(5) 0.033(5) 0.035(5) 0.005(4) 0.017(4) -0.008(4)
C5 0.040(5) 0.026(4) 0.030(4) 0.006(3) 0.010(4) -0.007(4)
C6 0.040(5) 0.031(4) 0.030(5) 0.010(4) 0.013(4) -0.009(4)
C7 0.052(5) 0.028(4) 0.028(4) 0.005(4) 0.010(4) -0.004(4)
C8 0.049(5) 0.027(4) 0.031(5) 0.008(4) 0.008(4) 0.000(4)
C9 0.043(5) 0.028(4) 0.033(5) 0.012(4) 0.009(4) -0.007(4)
C10 0.040(5) 0.025(4) 0.028(4) 0.008(3) 0.007(4) -0.007(4)
C11 0.052(6) 0.042(5) 0.043(5) 0.006(4) 0.012(5) 0.004(4)
C12 0.038(5) 0.031(5) 0.034(5) 0.011(4) 0.004(4) -0.009(4)
C13 0.050(6) 0.041(5) 0.039(5) 0.012(4) -0.008(4) -0.014(4)
C14 0.072(7) 0.038(5) 0.041(5) 0.015(4) 0.002(5) -0.007(5)
N5 0.051(5) 0.041(4) 0.028(4) 0.002(3) 0.007(3) -0.006(4)
N6 0.056(5) 0.046(5) 0.032(4) -0.003(4) -0.001(4) -0.003(4)
C15 0.052(6) 0.043(5) 0.041(5) -0.010(4) 0.011(5) -0.011(5)
C16 0.064(7) 0.045(6) 0.046(6) 0.003(5) 0.016(5) -0.007(5)
C17 0.078(8) 0.044(6) 0.048(6) 0.006(5) 0.023(6) -0.014(5)
C18 0.070(8) 0.051(6) 0.060(7) 0.000(5) 0.028(6) -0.027(6)
C19 0.052(6) 0.057(7) 0.055(7) -0.008(5) 0.021(5) -0.015(5)
C20 0.045(6) 0.046(6) 0.044(6) -0.007(4) 0.007(5) -0.003(5)
C21 0.076(8) 0.078(8) 0.045(6) 0.021(6) -0.004(6) -0.003(6)
C22 0.053(7) 0.105(10) 0.067(8) 0.033(7) -0.017(6) 0.003(7)
C23 0.061(8) 0.112(11) 0.078(9) 0.014(8) -0.012(7) 0.013(8)
C24 0.038(6) 0.078(8) 0.064(7) -0.009(6) 0.004(5) -0.001(5)
N7 0.052(5) 0.042(4) 0.030(4) 0.004(3) -0.003(4) -0.007(4)
N8 0.045(4) 0.041(4) 0.026(4) 0.005(3) 0.000(3) -0.001(3)
C25 0.061(6) 0.042(5) 0.030(5) 0.005(4) 0.006(4) -0.005(5)
C26 0.066(7) 0.037(5) 0.035(5) 0.004(4) -0.001(5) -0.011(5)
C27 0.099(9) 0.035(5) 0.049(6) 0.001(5) 0.003(6) -0.010(6)
C28 0.146(13) 0.039(6) 0.060(7) -0.012(5) 0.051(8) -0.009(7)
C29 0.104(10) 0.053(7) 0.044(6) 0.007(5) 0.032(6) -0.006(6)
C30 0.050(6) 0.044(5) 0.029(5) 0.009(4) 0.004(4) -0.002(4)
C31 0.071(7) 0.034(5) 0.032(5) 0.007(4) 0.004(5) -0.007(5)
C32 0.067(7) 0.039(5) 0.039(5) 0.013(4) -0.002(5) -0.008(5)
C33 0.062(6) 0.050(6) 0.040(5) 0.019(5) 0.003(5) -0.010(5)
C34 0.054(6) 0.053(6) 0.033(5) 0.014(4) 0.006(4) 0.005(5)
P1 0.069(2) 0.075(2) 0.0403(15) 0.0062(14) 0.0069(14) -0.0293(16)
P2 0.112(3) 0.062(2) 0.076(2) 0.0044(17) 0.032(2) -0.018(2)
P3 0.071(2) 0.086(2) 0.118(3) 0.060(2) 0.015(2) 0.0059(19)
O1S 0.31(3) 0.35(3) 0.173(18) 0.13(2) 0.057(18) -0.09(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
Ru1 N2 2.042(7) . ?
Ru1 N5 2.050(7) . ?
Ru1 N6 2.053(8) . ?
Ru1 N7 2.054(7) . ?
Ru1 N8 2.058(7) . ?
Ru1 N1 2.058(7) . ?
N1 C2 1.347(11) . ?
N1 C1 1.348(11) . ?
N2 C6 1.358(10) . ?
N2 C7 1.373(11) . ?
N3 C12 1.339(11) . ?
N3 C13 1.433(11) . ?
N4 C14 1.449(12) . ?
O1 C12 1.234(10) . ?
C1 C5 1.392(11) . ?
C1 C6 1.486(12) . ?
C2 C3 1.389(12) . ?
C3 C4 1.376(13) . ?
C4 C5 1.397(12) . ?
C4 C11 1.497(12) . ?
C6 C10 1.392(12) . ?
C7 C8 1.350(12) . ?
C8 C9 1.389(12) . ?
C9 C10 1.388(12) . ?
C9 C12 1.512(12) . ?
C13 C14 1.507(13) . ?
N5 C16 1.346(13) . ?
N5 C15 1.358(13) . ?
N6 C21 1.368(14) . ?
N6 C20 1.375(12) . ?
C15 C19 1.406(14) . ?
C15 C20 1.459(15) . ?
C16 C17 1.396(14) . ?
C17 C18 1.346(17) . ?
C18 C19 1.366(17) . ?
C20 C24 1.373(15) . ?
C21 C22 1.369(16) . ?
C22 C23 1.361(19) . ?
C23 C24 1.426(19) . ?
N7 C26 1.353(12) . ?
N7 C25 1.373(12) . ?
N8 C31 1.346(11) . ?
N8 C30 1.367(11) . ?
C25 C29 1.372(14) . ?
C25 C30 1.466(13) . ?
C26 C27 1.367(14) . ?
C27 C28 1.360(16) . ?
C28 C29 1.394(15) . ?
C30 C34 1.389(13) . ?
C31 C32 1.379(13) . ?
C32 C33 1.378(14) . ?
C33 C34 1.365(13) . ?
P1 O4' 1.352(18) . ?
P1 O3" 1.399(15) . ?
P1 O5" 1.445(17) . ?
P1 O2" 1.524(15) . ?
P1 O2' 1.528(16) . ?
P1 O3' 1.531(18) . ?
P1 O5' 1.60(2) . ?
P1 O4" 1.705(12) . ?
P2 O9' 1.404(11) . ?
P2 O7" 1.406(18) . ?
P2 O8' 1.570(14) . ?
P2 O6' 1.578(15) . ?
P2 O7' 1.603(15) . ?
P2 O6" 1.65(2) . ?
P2 O8" 1.67(3) . ?
P2 O9" 1.76(2) . ?
P3 O12' 1.42(3) . ?
P3 O10" 1.447(10) . ?
P3 O13' 1.49(4) . ?
P3 O11' 1.50(2) . ?
P3 O12" 1.527(15) . ?
P3 O11" 1.555(16) . ?
P3 O13" 1.585(16) . ?
P3 O10' 1.59(4) . ?
O1S C1S 1.343(14) . ?
C1S C2S' 1.474(18) . ?
C1S C3S' 1.49(2) . ?
C1S C2S" 1.506(18) . ?
C1S C3S" 1.528(18) . ?

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 Ru1 N5 94.7(3) . . ?
N2 Ru1 N6 171.4(3) . . ?
N5 Ru1 N6 78.7(3) . . ?
N2 Ru1 N7 93.5(3) . . ?
N5 Ru1 N7 97.1(3) . . ?
N6 Ru1 N7 92.8(3) . . ?
N2 Ru1 N8 91.2(3) . . ?
N5 Ru1 N8 173.2(3) . . ?
N6 Ru1 N8 95.8(3) . . ?
N7 Ru1 N8 79.0(3) . . ?
N2 Ru1 N1 78.5(3) . . ?
N5 Ru1 N1 88.8(3) . . ?
N6 Ru1 N1 95.6(3) . . ?
N7 Ru1 N1 170.6(3) . . ?
N8 Ru1 N1 95.9(3) . . ?
C2 N1 C1 116.9(7) . . ?
C2 N1 Ru1 126.7(6) . . ?
C1 N1 Ru1 116.3(5) . . ?
C6 N2 C7 116.5(7) . . ?
C6 N2 Ru1 116.7(6) . . ?
C7 N2 Ru1 126.8(6) . . ?
C12 N3 C13 122.6(8) . . ?
N1 C1 C5 122.4(8) . . ?
N1 C1 C6 114.3(7) . . ?
C5 C1 C6 123.3(8) . . ?
N1 C2 C3 123.9(9) . . ?
C4 C3 C2 119.0(9) . . ?
C3 C4 C5 117.9(8) . . ?
C3 C4 C11 120.8(8) . . ?
C5 C4 C11 121.3(8) . . ?
C1 C5 C4 119.9(8) . . ?
N2 C6 C10 122.9(8) . . ?
N2 C6 C1 114.0(7) . . ?
C10 C6 C1 123.0(7) . . ?
C8 C7 N2 122.9(8) . . ?
C7 C8 C9 120.8(8) . . ?
C10 C9 C8 117.7(8) . . ?
C10 C9 C12 124.2(7) . . ?
C8 C9 C12 118.0(8) . . ?
C9 C10 C6 119.2(7) . . ?
O1 C12 N3 122.7(8) . . ?
O1 C12 C9 119.2(7) . . ?
N3 C12 C9 118.1(8) . . ?
N3 C13 C14 113.3(8) . . ?
N4 C14 C13 112.5(8) . . ?
C16 N5 C15 118.1(9) . . ?
C16 N5 Ru1 126.1(7) . . ?
C15 N5 Ru1 115.8(7) . . ?
C21 N6 C20 118.2(9) . . ?
C21 N6 Ru1 126.2(8) . . ?
C20 N6 Ru1 115.6(7) . . ?
N5 C15 C19 121.2(10) . . ?
N5 C15 C20 115.2(9) . . ?
C19 C15 C20 123.5(10) . . ?
N5 C16 C17 122.1(11) . . ?
C18 C17 C16 119.4(11) . . ?
C17 C18 C19 120.3(10) . . ?
C18 C19 C15 118.9(11) . . ?
C24 C20 N6 120.4(11) . . ?
C24 C20 C15 125.3(10) . . ?
N6 C20 C15 114.3(9) . . ?
N6 C21 C22 123.3(12) . . ?
C23 C22 C21 119.3(13) . . ?
C22 C23 C24 118.6(12) . . ?
C20 C24 C23 120.2(12) . . ?
C26 N7 C25 117.6(8) . . ?
C26 N7 Ru1 126.8(6) . . ?
C25 N7 Ru1 115.4(6) . . ?
C31 N8 C30 117.7(8) . . ?
C31 N8 Ru1 126.5(6) . . ?
C30 N8 Ru1 115.8(6) . . ?
C29 C25 N7 121.5(9) . . ?
C29 C25 C30 123.7(9) . . ?
N7 C25 C30 114.9(8) . . ?
N7 C26 C27 122.1(9) . . ?
C28 C27 C26 120.9(10) . . ?
C27 C28 C29 117.9(10) . . ?
C25 C29 C28 120.0(10) . . ?
N8 C30 C34 121.1(8) . . ?
N8 C30 C25 114.6(8) . . ?
C34 C30 C25 124.2(8) . . ?
N8 C31 C32 122.8(9) . . ?
C33 C32 C31 119.2(9) . . ?
C34 C33 C32 118.9(9) . . ?
C33 C34 C30 120.2(9) . . ?
O4' P1 O3" 107.2(10) . . ?
O4' P1 O5" 55.9(9) . . ?
O3" P1 O5" 128.8(10) . . ?
O4' P1 O2" 109.7(10) . . ?
O3" P1 O2" 120.1(9) . . ?
O5" P1 O2" 110.9(9) . . ?
O4' P1 O2' 125.1(11) . . ?
O3" P1 O2' 115.8(10) . . ?
O5" P1 O2' 111.5(9) . . ?
O2" P1 O2' 17.2(8) . . ?
O4' P1 O3' 122.7(11) . . ?
O3" P1 O3' 16.1(9) . . ?
O5" P1 O3' 138.8(10) . . ?
O2" P1 O3' 107.4(10) . . ?
O2' P1 O3' 100.7(10) . . ?
O4' P1 O5' 109.7(11) . . ?
O3" P1 O5' 111.6(10) . . ?
O5" P1 O5' 54.0(9) . . ?
O2" P1 O5' 98.2(10) . . ?
O2' P1 O5' 85.1(10) . . ?
O3' P1 O5' 106.4(10) . . ?
O4' P1 O4" 45.6(8) . . ?
O3" P1 O4" 99.4(8) . . ?
O5" P1 O4" 96.2(8) . . ?
O2" P1 O4" 76.4(8) . . ?
O2' P1 O4" 93.5(8) . . ?
O3' P1 O4" 107.0(8) . . ?
O5' P1 O4" 146.2(8) . . ?
O9' P2 O7" 134.5(11) . . ?
O9' P2 O8' 112.6(7) . . ?
O7" P2 O8' 93.2(10) . . ?
O9' P2 O6' 110.8(7) . . ?
O7" P2 O6' 99.0(9) . . ?
O8' P2 O6' 101.5(9) . . ?
O9' P2 O7' 116.6(8) . . ?
O7" P2 O7' 18.7(9) . . ?
O8' P2 O7' 108.4(8) . . ?
O6' P2 O7' 105.7(8) . . ?
O9' P2 O6" 110.5(8) . . ?
O7" P2 O6" 106.4(11) . . ?
O8' P2 O6" 89.2(10) . . ?
O6' P2 O6" 13.9(9) . . ?
O7' P2 O6" 116.3(9) . . ?
O9' P2 O8" 104.9(13) . . ?
O7" P2 O8" 110.1(15) . . ?
O8' P2 O8" 20.3(12) . . ?
O6' P2 O8" 87.4(15) . . ?
O7' P2 O8" 127.0(13) . . ?
O6" P2 O8" 74.0(16) . . ?
O9' P2 O9" 39.1(8) . . ?
O7" P2 O9" 97.2(12) . . ?
O8' P2 O9" 138.4(9) . . ?
O6' P2 O9" 116.4(9) . . ?
O7' P2 O9" 78.6(9) . . ?
O6" P2 O9" 125.4(11) . . ?
O8" P2 O9" 140.6(14) . . ?
O12' P3 O10" 127.6(12) . . ?
O12' P3 O13' 113.5(19) . . ?
O10" P3 O13' 74.3(16) . . ?
O12' P3 O11' 96.5(15) . . ?
O10" P3 O11' 121.7(10) . . ?
O13' P3 O11' 125.2(18) . . ?
O12' P3 O12" 27.6(11) . . ?
O10" P3 O12" 111.7(7) . . ?
O13' P3 O12" 136.2(16) . . ?
O11' P3 O12" 89.7(12) . . ?
O12' P3 O11" 112.9(12) . . ?
O10" P3 O11" 112.9(7) . . ?
O13' P3 O11" 107.6(16) . . ?
O11' P3 O11" 19.2(10) . . ?
O12" P3 O11" 108.8(9) . . ?
O12' P3 O13" 79.2(13) . . ?
O10" P3 O13" 114.3(7) . . ?
O13' P3 O13" 41.9(14) . . ?
O11' P3 O13" 109.3(11) . . ?
O12" P3 O13" 106.7(9) . . ?
O11" P3 O13" 101.7(8) . . ?
O12' P3 O10' 97.4(18) . . ?
O10" P3 O10' 56.0(13) . . ?
O13' P3 O10' 130(2) . . ?
O11' P3 O10' 86.0(16) . . ?
O12" P3 O10' 70.2(14) . . ?
O11" P3 O10' 93.5(14) . . ?
O13" P3 O10' 164.6(14) . . ?
O1S C1S C2S' 130.8(19) . . ?
O1S C1S C3S' 128(2) . . ?
C2S' C1S C3S' 101(3) . . ?
O1S C1S C2S" 120.1(17) . . ?
C2S' C1S C2S" 31(2) . . ?
C3S' C1S C2S" 103(4) . . ?
O1S C1S C3S" 119.6(17) . . ?
C2S' C1S C3S" 98(3) . . ?
C3S' C1S C3S" 39(5) . . ?
C2S" C1S C3S" 120(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ru1 N1 C2 177.5(8) . . . . ?
N5 Ru1 N1 C2 -87.5(7) . . . . ?
N6 Ru1 N1 C2 -8.9(8) . . . . ?
N7 Ru1 N1 C2 144.1(16) . . . . ?
N8 Ru1 N1 C2 87.5(7) . . . . ?
N2 Ru1 N1 C1 0.1(6) . . . . ?
N5 Ru1 N1 C1 95.1(6) . . . . ?
N6 Ru1 N1 C1 173.7(6) . . . . ?
N7 Ru1 N1 C1 -33(2) . . . . ?
N8 Ru1 N1 C1 -89.9(6) . . . . ?
N5 Ru1 N2 C6 -85.7(6) . . . . ?
N6 Ru1 N2 C6 -46(2) . . . . ?
N7 Ru1 N2 C6 176.9(6) . . . . ?
N8 Ru1 N2 C6 97.9(6) . . . . ?
N1 Ru1 N2 C6 2.1(5) . . . . ?
N5 Ru1 N2 C7 90.1(7) . . . . ?
N6 Ru1 N2 C7 129.8(18) . . . . ?
N7 Ru1 N2 C7 -7.3(7) . . . . ?
N8 Ru1 N2 C7 -86.3(7) . . . . ?
N1 Ru1 N2 C7 177.9(7) . . . . ?
C2 N1 C1 C5 -0.1(12) . . . . ?
Ru1 N1 C1 C5 177.6(6) . . . . ?
C2 N1 C1 C6 -179.7(7) . . . . ?
Ru1 N1 C1 C6 -2.0(9) . . . . ?
C1 N1 C2 C3 -1.2(13) . . . . ?
Ru1 N1 C2 C3 -178.6(7) . . . . ?
N1 C2 C3 C4 2.6(14) . . . . ?
C2 C3 C4 C5 -2.5(13) . . . . ?
C2 C3 C4 C11 177.0(8) . . . . ?
N1 C1 C5 C4 0.0(12) . . . . ?
C6 C1 C5 C4 179.5(7) . . . . ?
C3 C4 C5 C1 1.3(12) . . . . ?
C11 C4 C5 C1 -178.2(8) . . . . ?
C7 N2 C6 C10 -1.4(11) . . . . ?
Ru1 N2 C6 C10 174.9(6) . . . . ?
C7 N2 C6 C1 -179.9(6) . . . . ?
Ru1 N2 C6 C1 -3.7(8) . . . . ?
N1 C1 C6 N2 3.7(10) . . . . ?
C5 C1 C6 N2 -175.9(7) . . . . ?
N1 C1 C6 C10 -174.9(7) . . . . ?
C5 C1 C6 C10 5.5(12) . . . . ?
C6 N2 C7 C8 1.5(11) . . . . ?
Ru1 N2 C7 C8 -174.3(6) . . . . ?
N2 C7 C8 C9 -0.5(13) . . . . ?
C7 C8 C9 C10 -0.8(12) . . . . ?
C7 C8 C9 C12 175.8(7) . . . . ?
C8 C9 C10 C6 0.9(11) . . . . ?
C12 C9 C10 C6 -175.4(7) . . . . ?
N2 C6 C10 C9 0.1(11) . . . . ?
C1 C6 C10 C9 178.6(7) . . . . ?
C13 N3 C12 O1 -3.0(13) . . . . ?
C13 N3 C12 C9 177.4(7) . . . . ?
C10 C9 C12 O1 171.4(8) . . . . ?
C8 C9 C12 O1 -4.9(11) . . . . ?
C10 C9 C12 N3 -8.9(12) . . . . ?
C8 C9 C12 N3 174.8(7) . . . . ?
C12 N3 C13 C14 -106.0(10) . . . . ?
N3 C13 C14 N4 63.8(11) . . . . ?
N2 Ru1 N5 C16 -8.6(7) . . . . ?
N6 Ru1 N5 C16 177.0(8) . . . . ?
N7 Ru1 N5 C16 85.5(7) . . . . ?
N8 Ru1 N5 C16 140(2) . . . . ?
N1 Ru1 N5 C16 -87.0(7) . . . . ?
N2 Ru1 N5 C15 168.9(6) . . . . ?
N6 Ru1 N5 C15 -5.5(6) . . . . ?
N7 Ru1 N5 C15 -96.9(6) . . . . ?
N8 Ru1 N5 C15 -43(3) . . . . ?
N1 Ru1 N5 C15 90.5(6) . . . . ?
N2 Ru1 N6 C21 142.2(17) . . . . ?
N5 Ru1 N6 C21 -177.3(9) . . . . ?
N7 Ru1 N6 C21 -80.7(8) . . . . ?
N8 Ru1 N6 C21 -1.5(9) . . . . ?
N1 Ru1 N6 C21 95.1(8) . . . . ?
N2 Ru1 N6 C20 -35(2) . . . . ?
N5 Ru1 N6 C20 5.2(6) . . . . ?
N7 Ru1 N6 C20 101.9(6) . . . . ?
N8 Ru1 N6 C20 -178.9(6) . . . . ?
N1 Ru1 N6 C20 -82.4(6) . . . . ?
C16 N5 C15 C19 0.7(12) . . . . ?
Ru1 N5 C15 C19 -177.1(7) . . . . ?
C16 N5 C15 C20 -177.4(8) . . . . ?
Ru1 N5 C15 C20 4.9(10) . . . . ?
C15 N5 C16 C17 -0.4(13) . . . . ?
Ru1 N5 C16 C17 177.1(7) . . . . ?
N5 C16 C17 C18 -0.3(15) . . . . ?
C16 C17 C18 C19 0.7(15) . . . . ?
C17 C18 C19 C15 -0.4(15) . . . . ?
N5 C15 C19 C18 -0.3(14) . . . . ?
C20 C15 C19 C18 177.6(9) . . . . ?
C21 N6 C20 C24 -0.3(13) . . . . ?
Ru1 N6 C20 C24 177.4(7) . . . . ?
C21 N6 C20 C15 178.1(8) . . . . ?
Ru1 N6 C20 C15 -4.2(10) . . . . ?
N5 C15 C20 C24 177.9(9) . . . . ?
C19 C15 C20 C24 0.0(15) . . . . ?
N5 C15 C20 N6 -0.4(11) . . . . ?
C19 C15 C20 N6 -178.4(8) . . . . ?
C20 N6 C21 C22 -0.5(16) . . . . ?
Ru1 N6 C21 C22 -177.8(9) . . . . ?
N6 C21 C22 C23 2.8(19) . . . . ?
C21 C22 C23 C24 -4(2) . . . . ?
N6 C20 C24 C23 -1.2(15) . . . . ?
C15 C20 C24 C23 -179.4(10) . . . . ?
C22 C23 C24 C20 3.5(18) . . . . ?
N2 Ru1 N7 C26 88.8(8) . . . . ?
N5 Ru1 N7 C26 -6.4(8) . . . . ?
N6 Ru1 N7 C26 -85.4(8) . . . . ?
N8 Ru1 N7 C26 179.3(8) . . . . ?
N1 Ru1 N7 C26 121.5(17) . . . . ?
N2 Ru1 N7 C25 -84.8(7) . . . . ?
N5 Ru1 N7 C25 180.0(7) . . . . ?
N6 Ru1 N7 C25 101.0(7) . . . . ?
N8 Ru1 N7 C25 5.6(6) . . . . ?
N1 Ru1 N7 C25 -52(2) . . . . ?
N2 Ru1 N8 C31 -91.9(8) . . . . ?
N5 Ru1 N8 C31 120(2) . . . . ?
N6 Ru1 N8 C31 83.1(8) . . . . ?
N7 Ru1 N8 C31 174.8(8) . . . . ?
N1 Ru1 N8 C31 -13.3(8) . . . . ?
N2 Ru1 N8 C30 90.0(6) . . . . ?
N5 Ru1 N8 C30 -59(3) . . . . ?
N6 Ru1 N8 C30 -95.1(6) . . . . ?
N7 Ru1 N8 C30 -3.4(6) . . . . ?
N1 Ru1 N8 C30 168.6(6) . . . . ?
C26 N7 C25 C29 -2.3(15) . . . . ?
Ru1 N7 C25 C29 171.9(9) . . . . ?
C26 N7 C25 C30 178.9(8) . . . . ?
Ru1 N7 C25 C30 -6.9(11) . . . . ?
C25 N7 C26 C27 1.4(14) . . . . ?
Ru1 N7 C26 C27 -172.1(8) . . . . ?
N7 C26 C27 C28 1.3(18) . . . . ?
C26 C27 C28 C29 -3(2) . . . . ?
N7 C25 C29 C28 0.6(19) . . . . ?
C30 C25 C29 C28 179.3(12) . . . . ?
C27 C28 C29 C25 2(2) . . . . ?
C31 N8 C30 C34 1.9(13) . . . . ?
Ru1 N8 C30 C34 -179.7(7) . . . . ?
C31 N8 C30 C25 -177.5(8) . . . . ?
Ru1 N8 C30 C25 0.8(10) . . . . ?
C29 C25 C30 N8 -174.8(10) . . . . ?
N7 C25 C30 N8 4.0(12) . . . . ?
C29 C25 C30 C34 5.7(16) . . . . ?
N7 C25 C30 C34 -175.4(9) . . . . ?
C30 N8 C31 C32 -1.2(14) . . . . ?
Ru1 N8 C31 C32 -179.4(7) . . . . ?
N8 C31 C32 C33 0.1(15) . . . . ?
C31 C32 C33 C34 0.3(15) . . . . ?
C32 C33 C34 C30 0.4(15) . . . . ?
N8 C30 C34 C33 -1.6(14) . . . . ?
C25 C30 C34 C33 177.8(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        23.25
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.516
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.152

#===END

data_L1
_database_code_depnum_ccdc_archive 'CCDC 263037'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_publ_section_exptl_refinement   
;
The structure was solved by direct methods.
Data processing was carried out to 0.75 angstroms
(although it was only complete to 0.8 angstroms).
Restraints were used on the anisotropic thermal
parameters of the atoms C15 N4 O2 and
O3. It was not possible to determine
the absolute configuration. Hydrogens were
included in calculated positions using the riding model.
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H24 N4 O3'
_chemical_formula_weight         356.42

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   5.0564(15)
_cell_length_b                   5.6297(18)
_cell_length_c                   16.199(5)
_cell_angle_alpha                87.396(5)
_cell_angle_beta                 83.943(5)
_cell_angle_gamma                84.685(6)
_cell_volume                     456.3(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2838
_cell_measurement_theta_min      2.535
_cell_measurement_theta_max      26.152

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             190
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9736
_exptl_absorpt_correction_T_max  0.9991
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'CCD area'
_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            2838
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         28.41
_reflns_number_total             2011
_reflns_number_gt                1610
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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^)+(0.1001P)^2^+0.4217P] 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       ?
_chemical_absolute_configuration unk
_refine_ls_number_reflns         2011
_refine_ls_number_parameters     239
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0716
_refine_ls_wR_factor_ref         0.2006
_refine_ls_wR_factor_gt          0.1804
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.090
_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
N1 N 0.9888(9) 1.0413(7) -0.2302(3) 0.0233(10) Uani 1 1 d . . .
C1 C 0.8327(11) 1.2443(9) -0.2386(3) 0.0208(11) Uani 1 1 d . . .
O1 O 0.0356(8) 0.9599(7) 0.0432(3) 0.0335(10) Uani 1 1 d . . .
N2 N 0.4404(9) 1.4862(7) -0.1852(3) 0.0231(10) Uani 1 1 d . . .
C2 C 1.2009(12) 1.0026(9) -0.2852(3) 0.0266(12) Uani 1 1 d . . .
H2 H 1.3092 0.8612 -0.2797 0.032 Uiso 1 1 calc R . .
O2 O 0.9163(15) 0.3189(9) 0.2298(3) 0.0663(15) Uani 1 1 d U . .
N3 N 0.4759(9) 0.9007(8) 0.0569(3) 0.0250(10) Uani 1 1 d . . .
H3N H 0.6341 0.9250 0.0352 0.030 Uiso 1 1 calc R . .
C3 C 1.2701(11) 1.1598(9) -0.3501(3) 0.0246(12) Uani 1 1 d . . .
H3 H 1.4228 1.1256 -0.3863 0.030 Uiso 1 1 calc R . .
O3 O 0.5803(11) 0.1473(8) 0.3102(3) 0.0456(12) Uani 1 1 d U . .
N4 N 0.4846(18) 0.3616(10) 0.1984(3) 0.0646(17) Uani 1 1 d U . .
H4N H 0.3245 0.3276 0.2145 0.077 Uiso 1 1 calc R . .
C4 C 1.1078(11) 1.3706(9) -0.3605(3) 0.0237(12) Uani 1 1 d . . .
C5 C 0.8887(11) 1.4121(9) -0.3034(3) 0.0225(11) Uani 1 1 d . . .
H5 H 0.7771 1.5520 -0.3077 0.027 Uiso 1 1 calc R . .
C6 C 0.5998(11) 1.2869(9) -0.1753(3) 0.0206(11) Uani 1 1 d . . .
C7 C 0.2274(11) 1.5249(9) -0.1305(3) 0.0242(12) Uani 1 1 d . . .
H7 H 0.1163 1.6642 -0.1369 0.029 Uiso 1 1 calc R . .
C8 C 0.1615(10) 1.3686(9) -0.0641(3) 0.0217(11) Uani 1 1 d . . .
H8 H 0.0080 1.4003 -0.0279 0.026 Uiso 1 1 calc R . .
C9 C 0.3320(11) 1.1634(9) -0.0533(3) 0.0214(12) Uani 1 1 d . . .
C10 C 0.5555(11) 1.1212(9) -0.1098(3) 0.0220(11) Uani 1 1 d . . .
H10 H 0.6731 0.9858 -0.1041 0.026 Uiso 1 1 calc R . .
C11 C 1.1806(13) 1.5480(10) -0.4293(4) 0.0303(14) Uani 1 1 d . . .
H11A H 1.0403 1.6748 -0.4306 0.045 Uiso 1 1 calc R . .
H11B H 1.2046 1.4702 -0.4814 0.045 Uiso 1 1 calc R . .
H11C H 1.3436 1.6124 -0.4197 0.045 Uiso 1 1 calc R . .
C12 C 0.2679(11) 0.9965(9) 0.0201(3) 0.0225(11) Uani 1 1 d . . .
C13 C 0.4434(12) 0.7547(10) 0.1334(3) 0.0281(12) Uani 1 1 d . . .
H13A H 0.5432 0.8166 0.1744 0.034 Uiso 1 1 calc R . .
H13B H 0.2564 0.7677 0.1550 0.034 Uiso 1 1 calc R . .
C14 C 0.533(2) 0.5050(11) 0.1221(4) 0.068(3) Uani 1 1 d . . .
H14A H 0.7226 0.4903 0.1038 0.081 Uiso 1 1 calc R . .
H14B H 0.4404 0.4445 0.0791 0.081 Uiso 1 1 calc R . .
C15 C 0.682(2) 0.2809(11) 0.2444(4) 0.0564(15) Uani 1 1 d U . .
C16 C 0.7592(15) 0.0306(10) 0.3679(4) 0.0373(15) Uani 1 1 d . . .
C17 C 0.8751(13) 0.2158(10) 0.4143(4) 0.0340(14) Uani 1 1 d . . .
H17A H 1.0118 0.2873 0.3785 0.051 Uiso 1 1 calc R . .
H17B H 0.9506 0.1415 0.4620 0.051 Uiso 1 1 calc R . .
H17C H 0.7367 0.3367 0.4320 0.051 Uiso 1 1 calc R . .
C18 C 0.5718(14) -0.1061(12) 0.4276(4) 0.0387(15) Uani 1 1 d . . .
H18A H 0.4343 0.0033 0.4535 0.058 Uiso 1 1 calc R . .
H18B H 0.6701 -0.1887 0.4694 0.058 Uiso 1 1 calc R . .
H18C H 0.4923 -0.2195 0.3976 0.058 Uiso 1 1 calc R . .
C19 C 0.9678(17) -0.1421(11) 0.3236(5) 0.050(2) Uani 1 1 d . . .
H19A H 0.8849 -0.2334 0.2866 0.075 Uiso 1 1 calc R . .
H19B H 1.0494 -0.2478 0.3637 0.075 Uiso 1 1 calc R . .
H19C H 1.1017 -0.0548 0.2925 0.075 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
N1 0.030(3) 0.019(2) 0.022(2) 0.0040(17) -0.005(2) -0.0020(19)
C1 0.024(3) 0.019(2) 0.020(3) 0.0038(19) -0.004(2) -0.008(2)
O1 0.033(2) 0.035(2) 0.032(2) 0.0098(17) 0.0029(18) -0.0066(18)
N2 0.029(3) 0.020(2) 0.020(2) 0.0049(17) -0.004(2) -0.0045(19)
C2 0.035(3) 0.020(3) 0.024(3) 0.000(2) -0.001(2) 0.003(2)
O2 0.142(4) 0.032(2) 0.028(2) 0.0038(19) 0.007(3) -0.049(3)
N3 0.029(2) 0.021(2) 0.023(2) 0.0081(17) -0.0020(18) 0.0006(18)
C3 0.028(3) 0.022(3) 0.024(3) 0.001(2) -0.001(2) -0.004(2)
O3 0.089(4) 0.025(2) 0.025(2) 0.0096(15) -0.009(2) -0.017(2)
N4 0.155(5) 0.021(3) 0.020(2) 0.0084(18) -0.010(3) -0.018(3)
C4 0.036(3) 0.021(3) 0.016(2) 0.003(2) -0.008(2) -0.008(2)
C5 0.027(3) 0.018(2) 0.024(3) 0.0059(19) -0.007(2) -0.007(2)
C6 0.024(3) 0.017(2) 0.021(3) 0.0077(19) -0.005(2) -0.005(2)
C7 0.028(3) 0.020(3) 0.025(3) 0.004(2) -0.008(2) -0.002(2)
C8 0.017(3) 0.023(3) 0.025(3) 0.000(2) 0.000(2) -0.002(2)
C9 0.023(3) 0.021(3) 0.021(3) 0.001(2) -0.005(2) -0.007(2)
C10 0.026(3) 0.018(2) 0.022(3) 0.004(2) -0.005(2) 0.000(2)
C11 0.043(4) 0.026(3) 0.022(3) 0.005(2) 0.004(3) -0.010(3)
C12 0.026(3) 0.018(2) 0.023(3) 0.001(2) -0.001(2) -0.002(2)
C13 0.036(3) 0.025(3) 0.020(3) 0.008(2) 0.002(2) 0.003(2)
C14 0.165(10) 0.021(3) 0.015(3) 0.006(2) -0.002(4) -0.010(4)
C15 0.133(4) 0.015(3) 0.025(3) 0.0042(19) -0.005(3) -0.032(3)
C16 0.066(5) 0.018(3) 0.027(3) 0.004(2) 0.004(3) -0.012(3)
C17 0.045(4) 0.025(3) 0.030(3) -0.003(2) 0.004(3) 0.002(3)
C18 0.041(4) 0.038(3) 0.035(3) 0.016(3) -0.002(3) -0.004(3)
C19 0.080(5) 0.024(3) 0.044(4) -0.005(3) 0.022(4) -0.023(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
N1 C2 1.328(7) . ?
N1 C1 1.338(7) . ?
C1 C5 1.404(6) . ?
C1 C6 1.487(6) . ?
O1 C12 1.228(7) . ?
N2 C7 1.329(7) . ?
N2 C6 1.333(7) . ?
C2 C3 1.380(7) . ?
C2 H2 0.9300 . ?
O2 C15 1.219(12) . ?
N3 C12 1.323(7) . ?
N3 C13 1.459(6) . ?
N3 H3N 0.8600 . ?
C3 C4 1.393(8) . ?
C3 H3 0.9300 . ?
O3 C15 1.360(7) . ?
O3 C16 1.462(8) . ?
N4 C15 1.342(12) . ?
N4 C14 1.456(7) . ?
N4 H4N 0.8600 . ?
C4 C5 1.376(8) . ?
C4 C11 1.501(7) . ?
C5 H5 0.9300 . ?
C6 C10 1.395(7) . ?
C7 C8 1.390(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.392(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(8) . ?
C9 C12 1.508(7) . ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C13 C14 1.450(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16 C17 1.508(8) . ?
C16 C19 1.512(10) . ?
C16 C18 1.516(8) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

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
C2 N1 C1 117.9(4) . . ?
N1 C1 C5 121.5(5) . . ?
N1 C1 C6 117.1(4) . . ?
C5 C1 C6 121.4(4) . . ?
C7 N2 C6 117.9(4) . . ?
N1 C2 C3 123.9(5) . . ?
N1 C2 H2 118.1 . . ?
C3 C2 H2 118.1 . . ?
C12 N3 C13 121.6(5) . . ?
C12 N3 H3N 119.2 . . ?
C13 N3 H3N 119.2 . . ?
C2 C3 C4 119.0(5) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C15 O3 C16 119.5(6) . . ?
C15 N4 C14 122.0(9) . . ?
C15 N4 H4N 119.0 . . ?
C14 N4 H4N 119.0 . . ?
C5 C4 C3 117.2(5) . . ?
C5 C4 C11 122.3(5) . . ?
C3 C4 C11 120.4(5) . . ?
C4 C5 C1 120.4(5) . . ?
C4 C5 H5 119.8 . . ?
C1 C5 H5 119.8 . . ?
N2 C6 C10 123.1(5) . . ?
N2 C6 C1 116.9(4) . . ?
C10 C6 C1 120.0(4) . . ?
N2 C7 C8 123.6(5) . . ?
N2 C7 H7 118.2 . . ?
C8 C7 H7 118.2 . . ?
C7 C8 C9 118.1(5) . . ?
C7 C8 H8 121.0 . . ?
C9 C8 H8 121.0 . . ?
C10 C9 C8 118.9(5) . . ?
C10 C9 C12 122.5(5) . . ?
C8 C9 C12 118.6(5) . . ?
C9 C10 C6 118.4(5) . . ?
C9 C10 H10 120.8 . . ?
C6 C10 H10 120.8 . . ?
C4 C11 H11A 109.5 . . ?
C4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1 C12 N3 124.1(5) . . ?
O1 C12 C9 120.5(5) . . ?
N3 C12 C9 115.4(5) . . ?
C14 C13 N3 113.1(5) . . ?
C14 C13 H13A 109.0 . . ?
N3 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
N3 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C13 C14 N4 111.9(5) . . ?
C13 C14 H14A 109.2 . . ?
N4 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
N4 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
O2 C15 N4 125.9(6) . . ?
O2 C15 O3 125.0(8) . . ?
N4 C15 O3 109.1(8) . . ?
O3 C16 C17 109.9(5) . . ?
O3 C16 C19 111.0(5) . . ?
C17 C16 C19 113.6(6) . . ?
O3 C16 C18 102.6(5) . . ?
C17 C16 C18 109.5(5) . . ?
C19 C16 C18 109.7(5) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 C5 0.2(8) . . . . ?
C2 N1 C1 C6 -178.6(5) . . . . ?
C1 N1 C2 C3 0.3(8) . . . . ?
N1 C2 C3 C4 -1.2(9) . . . . ?
C2 C3 C4 C5 1.5(8) . . . . ?
C2 C3 C4 C11 178.6(5) . . . . ?
C3 C4 C5 C1 -1.0(7) . . . . ?
C11 C4 C5 C1 -178.0(5) . . . . ?
N1 C1 C5 C4 0.2(8) . . . . ?
C6 C1 C5 C4 179.0(5) . . . . ?
C7 N2 C6 C10 -1.2(8) . . . . ?
C7 N2 C6 C1 178.4(5) . . . . ?
N1 C1 C6 N2 -178.2(5) . . . . ?
C5 C1 C6 N2 3.0(7) . . . . ?
N1 C1 C6 C10 1.4(7) . . . . ?
C5 C1 C6 C10 -177.4(5) . . . . ?
C6 N2 C7 C8 -0.4(8) . . . . ?
N2 C7 C8 C9 1.7(8) . . . . ?
C7 C8 C9 C10 -1.3(8) . . . . ?
C7 C8 C9 C12 178.0(5) . . . . ?
C8 C9 C10 C6 -0.1(8) . . . . ?
C12 C9 C10 C6 -179.4(5) . . . . ?
N2 C6 C10 C9 1.5(8) . . . . ?
C1 C6 C10 C9 -178.1(5) . . . . ?
C13 N3 C12 O1 -4.9(8) . . . . ?
C13 N3 C12 C9 173.9(5) . . . . ?
C10 C9 C12 O1 -143.2(6) . . . . ?
C8 C9 C12 O1 37.6(8) . . . . ?
C10 C9 C12 N3 38.1(7) . . . . ?
C8 C9 C12 N3 -141.2(5) . . . . ?
C12 N3 C13 C14 111.3(7) . . . . ?
N3 C13 C14 N4 -176.8(7) . . . . ?
C15 N4 C14 C13 -104.9(9) . . . . ?
C14 N4 C15 O2 1.4(10) . . . . ?
C14 N4 C15 O3 -178.2(5) . . . . ?
C16 O3 C15 O2 -2.1(9) . . . . ?
C16 O3 C15 N4 177.5(5) . . . . ?
C15 O3 C16 C17 66.4(7) . . . . ?
C15 O3 C16 C19 -60.2(6) . . . . ?
C15 O3 C16 C18 -177.2(5) . . . . ?

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 H3N O1 0.86 2.08 2.864(6) 152.2 1_655
N4 H4N O2 0.86 2.06 2.895(12) 164.4 1_455

_diffrn_measured_fraction_theta_max 0.875
_diffrn_reflns_theta_full        28.41
_diffrn_measured_fraction_theta_full 0.875
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.086