# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Isabel Santos'
_publ_contact_author_email       ISANTOS@ITN.PT

_publ_section_title              
;
Rhenium and Technetium Complexes Bearing
Quinazoline Derivatives: Progress Towards a 99mTc Biomarker
for EGFR-TK Imaging.
;
loop_
_publ_author_name
'Isabel Santos'
'Athanasia Bourkoula'
'Aris Chiotellis'
'Celia Fernandes'
'Werner Kraus'
;
J.-U.Kunstler
;
'Nikos Margaritis'
'Maria Paravatou-Petsotas'
'Hans-Jurgen Pietzsch'
;
I.Pirmettis
;
'Ana Ray'

# Attachment 'Re_complex_8_ref.cif'

data_rhenium_complex_8
_database_code_depnum_ccdc_archive 'CCDC 676393'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H28 Br N6 O2 Re S3'
_chemical_formula_weight         794.81

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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                   7.806(11)
_cell_length_b                   11.379(19)
_cell_length_c                   16.234(17)
_cell_angle_alpha                91.294(19)
_cell_angle_beta                 91.37(3)
_cell_angle_gamma                105.35(2)
_cell_volume                     1389(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    2543
_cell_measurement_theta_min      2.515
_cell_measurement_theta_max      23.685

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_absorpt_coefficient_mu    6.071
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_T_max  0.374
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(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  SMART-APEX
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6811
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4231
_reflns_number_gt                3318
_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^)+(0.0648P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4231
_refine_ls_number_parameters     322
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1149
_refine_ls_wR_factor_gt          0.1007
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_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
Re1 Re 0.05622(5) 1.01604(3) 0.29955(2) 0.03598(16) Uani 1 1 d . . .
Br1 Br 0.23071(19) 1.57745(13) 0.47794(7) 0.0756(4) Uani 1 1 d . . .
S1 S 0.1169(4) 0.8417(2) 0.33467(17) 0.0559(7) Uani 1 1 d . . .
S2 S -0.0635(4) 1.1179(3) 0.39110(18) 0.0560(7) Uani 1 1 d . . .
S3 S 0.1807(4) 1.1088(2) 0.18647(15) 0.0479(6) Uani 1 1 d . . .
N1 N 0.3154(10) 1.1087(7) 0.3615(5) 0.047(2) Uani 1 1 d . . .
N2 N -0.3096(12) 0.8927(9) 0.2101(6) 0.068(3) Uani 1 1 d . . .
N3 N -0.1663(10) 1.0818(7) -0.0085(5) 0.046(2) Uani 1 1 d . . .
H3A H -0.1629 1.0262 -0.0447 0.055 Uiso 1 1 calc R . .
N4 N 0.2683(11) 1.5439(7) -0.0833(5) 0.045(2) Uani 1 1 d . . .
N5 N 0.3569(11) 1.5829(7) 0.0594(5) 0.045(2) Uani 1 1 d . . .
N6 N 0.2141(10) 1.4581(7) 0.1628(5) 0.0428(19) Uani 1 1 d . . .
H6A H 0.1227 1.4001 0.1740 0.051 Uiso 1 1 calc R . .
O1 O -0.2919(10) 1.1193(6) 0.1108(4) 0.0558(19) Uani 1 1 d . . .
C1 C 0.4290(17) 1.0242(11) 0.3654(8) 0.074(3) Uani 1 1 d . . .
H1A H 0.5254 1.0570 0.4052 0.089 Uiso 1 1 calc R . .
H1B H 0.4811 1.0209 0.3120 0.089 Uiso 1 1 calc R . .
C2 C 0.3364(16) 0.8971(11) 0.3883(8) 0.074(3) Uani 1 1 d . . .
H2B H 0.3208 0.8950 0.4474 0.089 Uiso 1 1 calc R . .
H2C H 0.4098 0.8433 0.3743 0.089 Uiso 1 1 calc R . .
C3 C 0.2828(16) 1.1480(12) 0.4474(7) 0.075(3) Uani 1 1 d . . .
H3B H 0.2598 1.0775 0.4820 0.090 Uiso 1 1 calc R . .
H3C H 0.3900 1.2059 0.4690 0.090 Uiso 1 1 calc R . .
C4 C 0.1327(16) 1.2044(12) 0.4534(8) 0.075(3) Uani 1 1 d . . .
H4B H 0.1697 1.2873 0.4345 0.090 Uiso 1 1 calc R . .
H4C H 0.1006 1.2077 0.5106 0.090 Uiso 1 1 calc R . .
C5 C 0.4038(16) 1.2182(11) 0.3186(7) 0.066(2) Uani 1 1 d . . .
H5B H 0.5257 1.2471 0.3394 0.079 Uiso 1 1 calc R . .
H5C H 0.3446 1.2814 0.3302 0.079 Uiso 1 1 calc R . .
C6 C 0.4034(15) 1.1961(11) 0.2245(7) 0.066(2) Uani 1 1 d . . .
H6B H 0.4897 1.1514 0.2114 0.079 Uiso 1 1 calc R . .
H6C H 0.4371 1.2737 0.1975 0.079 Uiso 1 1 calc R . .
C7 C -0.1687(14) 0.9412(9) 0.2419(6) 0.051(3) Uani 1 1 d . . .
C8 C -0.4380(13) 0.8743(9) 0.1430(7) 0.052(3) Uani 1 1 d . . .
H8A H -0.5232 0.9205 0.1546 0.063 Uiso 1 1 calc R . .
H8B H -0.5021 0.7887 0.1388 0.063 Uiso 1 1 calc R . .
C9 C -0.3535(12) 0.9130(9) 0.0608(6) 0.042(2) Uani 1 1 d . . .
H9A H -0.2642 0.8696 0.0505 0.050 Uiso 1 1 calc R . .
H9B H -0.4439 0.8901 0.0171 0.050 Uiso 1 1 calc R . .
C10 C -0.2702(12) 1.0451(9) 0.0588(6) 0.044(2) Uani 1 1 d . . .
C11 C -0.0634(12) 1.2038(9) -0.0241(6) 0.040(2) Uani 1 1 d . . .
C12 C -0.0480(12) 1.2392(9) -0.1056(6) 0.041(2) Uani 1 1 d . . .
H12A H -0.1104 1.1874 -0.1477 0.049 Uiso 1 1 calc R . .
C13 C 0.0600(13) 1.3511(10) -0.1231(6) 0.046(3) Uani 1 1 d . . .
H13A H 0.0700 1.3740 -0.1778 0.055 Uiso 1 1 calc R . .
C14 C 0.1556(12) 1.4320(8) -0.0623(6) 0.040(2) Uani 1 1 d . . .
C15 C 0.1365(12) 1.3963(8) 0.0200(5) 0.036(2) Uani 1 1 d . . .
C16 C 0.0249(11) 1.2809(8) 0.0379(6) 0.036(2) Uani 1 1 d . . .
H16A H 0.0114 1.2572 0.0923 0.043 Uiso 1 1 calc R . .
C17 C 0.3615(14) 1.6080(9) -0.0223(6) 0.048(3) Uani 1 1 d . . .
H17A H 0.4417 1.6804 -0.0364 0.057 Uiso 1 1 calc R . .
C18 C 0.2405(13) 1.4828(8) 0.0810(6) 0.038(2) Uani 1 1 d . . .
C19 C 0.3221(12) 1.5184(8) 0.2309(6) 0.039(2) Uani 1 1 d . . .
C20 C 0.5036(13) 1.5625(10) 0.2283(6) 0.053(3) Uani 1 1 d . . .
H20A H 0.5599 1.5608 0.1786 0.063 Uiso 1 1 calc R . .
C21 C 0.6037(16) 1.6097(11) 0.2990(8) 0.068(3) Uani 1 1 d . . .
H21A H 0.7262 1.6399 0.2957 0.081 Uiso 1 1 calc R . .
C22 C 0.5267(15) 1.6127(10) 0.3727(7) 0.060(3) Uani 1 1 d . . .
H22A H 0.5952 1.6428 0.4200 0.071 Uiso 1 1 calc R . .
C23 C 0.3449(15) 1.5700(9) 0.3758(6) 0.050(3) Uani 1 1 d . . .
C24 C 0.2396(13) 1.5229(9) 0.3055(6) 0.044(2) Uani 1 1 d . . .
H24A H 0.1167 1.4952 0.3086 0.053 Uiso 1 1 calc R . .
O4 O 0.1399(11) 1.6570(8) -0.2232(5) 0.069(2) Uani 1 1 d D . .
H4D H 0.155(16) 1.735(7) -0.194(7) 0.083 Uiso 1 1 d D . .
H4E H 0.187(16) 1.621(9) -0.177(6) 0.083 Uiso 1 1 d D . .

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
Re1 0.0372(2) 0.0371(2) 0.0313(2) -0.00778(15) -0.00679(15) 0.00703(16)
Br1 0.0863(9) 0.0893(9) 0.0415(7) -0.0092(6) 0.0102(6) 0.0067(7)
S1 0.0740(19) 0.0438(15) 0.0483(16) -0.0071(12) -0.0176(14) 0.0155(14)
S2 0.0453(15) 0.0666(18) 0.0546(17) -0.0157(14) 0.0058(12) 0.0130(14)
S3 0.0541(15) 0.0515(16) 0.0371(14) -0.0038(11) -0.0021(11) 0.0127(13)
N1 0.039(5) 0.041(5) 0.059(6) -0.016(4) -0.012(4) 0.010(4)
N2 0.052(6) 0.064(6) 0.072(7) -0.006(5) -0.026(5) -0.008(5)
N3 0.047(5) 0.040(5) 0.044(5) -0.017(4) -0.007(4) 0.002(4)
N4 0.053(5) 0.049(5) 0.036(5) -0.001(4) 0.007(4) 0.018(4)
N5 0.053(5) 0.039(5) 0.041(5) -0.010(4) -0.004(4) 0.008(4)
N6 0.043(5) 0.044(5) 0.035(5) -0.012(4) -0.007(4) 0.003(4)
O1 0.063(5) 0.043(4) 0.058(5) -0.016(4) 0.013(4) 0.008(4)
C1 0.070(6) 0.073(6) 0.082(7) -0.008(5) -0.027(5) 0.028(5)
C2 0.070(6) 0.073(6) 0.082(7) -0.008(5) -0.027(5) 0.028(5)
C3 0.065(5) 0.091(7) 0.063(6) -0.039(5) -0.004(4) 0.014(5)
C4 0.065(5) 0.091(7) 0.063(6) -0.039(5) -0.004(4) 0.014(5)
C5 0.055(5) 0.061(5) 0.072(6) -0.004(4) 0.003(4) 0.000(4)
C6 0.055(5) 0.061(5) 0.072(6) -0.004(4) 0.003(4) 0.000(4)
C7 0.050(6) 0.045(6) 0.050(7) 0.000(5) -0.016(5) 0.004(5)
C8 0.036(5) 0.049(6) 0.065(7) -0.013(5) -0.022(5) 0.005(5)
C9 0.035(5) 0.050(6) 0.039(6) -0.010(4) -0.008(4) 0.012(5)
C10 0.035(5) 0.047(6) 0.051(6) -0.021(5) -0.014(5) 0.017(5)
C11 0.032(5) 0.047(6) 0.045(6) -0.019(5) -0.004(4) 0.019(5)
C12 0.039(5) 0.054(6) 0.032(5) -0.013(4) -0.007(4) 0.016(5)
C13 0.050(6) 0.063(7) 0.032(5) -0.015(5) -0.008(4) 0.030(6)
C14 0.040(5) 0.044(6) 0.039(6) -0.009(4) 0.000(4) 0.018(5)
C15 0.036(5) 0.042(6) 0.033(5) -0.010(4) -0.003(4) 0.017(4)
C16 0.035(5) 0.039(5) 0.032(5) -0.007(4) -0.005(4) 0.009(4)
C17 0.053(6) 0.043(6) 0.045(6) -0.013(5) 0.004(5) 0.010(5)
C18 0.046(6) 0.038(6) 0.036(6) -0.010(4) -0.008(4) 0.021(5)
C19 0.045(6) 0.037(5) 0.037(5) -0.008(4) -0.004(4) 0.015(5)
C20 0.040(6) 0.070(7) 0.045(6) -0.018(5) -0.004(5) 0.013(5)
C21 0.051(7) 0.081(9) 0.069(8) -0.028(7) -0.005(6) 0.014(6)
C22 0.056(7) 0.069(8) 0.049(7) -0.022(6) -0.018(5) 0.013(6)
C23 0.066(7) 0.050(6) 0.034(6) -0.005(5) 0.000(5) 0.016(6)
C24 0.039(5) 0.049(6) 0.044(6) -0.006(5) -0.005(4) 0.011(5)
O4 0.065(5) 0.075(6) 0.062(5) -0.009(4) 0.003(4) 0.012(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C7 1.944(10) . ?
Re1 N1 2.223(8) . ?
Re1 S2 2.234(3) . ?
Re1 S1 2.241(4) . ?
Re1 S3 2.249(3) . ?
Br1 C23 1.912(10) . ?
S1 C2 1.851(12) . ?
S2 C4 1.849(12) . ?
S3 C6 1.843(11) . ?
N1 C5 1.457(14) . ?
N1 C1 1.471(14) . ?
N1 C3 1.503(13) . ?
N2 C7 1.191(13) . ?
N2 C8 1.435(12) . ?
N3 C10 1.382(13) . ?
N3 C11 1.439(12) . ?
N3 H3A 0.8600 . ?
N4 C17 1.301(12) . ?
N4 C14 1.397(12) . ?
N5 C18 1.316(12) . ?
N5 C17 1.363(12) . ?
N6 C18 1.373(12) . ?
N6 C19 1.421(11) . ?
N6 H6A 0.8600 . ?
O1 C10 1.227(11) . ?
C1 C2 1.495(17) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C3 C4 1.481(17) . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C5 C6 1.542(16) . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C8 C9 1.525(14) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.473(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C16 1.366(12) . ?
C11 C12 1.389(13) . ?
C12 C13 1.369(14) . ?
C12 H12A 0.9300 . ?
C13 C14 1.391(13) . ?
C13 H13A 0.9300 . ?
C14 C15 1.406(13) . ?
C15 C16 1.411(13) . ?
C15 C18 1.449(12) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?
C19 C20 1.374(14) . ?
C19 C24 1.391(13) . ?
C20 C21 1.386(14) . ?
C20 H20A 0.9300 . ?
C21 C22 1.356(15) . ?
C21 H21A 0.9300 . ?
C22 C23 1.376(15) . ?
C22 H22A 0.9300 . ?
C23 C24 1.400(13) . ?
C24 H24A 0.9300 . ?
O4 H4D 0.97(8) . ?
O4 H4E 0.98(8) . ?

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
C7 Re1 N1 177.4(4) . . ?
C7 Re1 S2 94.2(3) . . ?
N1 Re1 S2 85.9(2) . . ?
C7 Re1 S1 96.4(3) . . ?
N1 Re1 S1 85.8(2) . . ?
S2 Re1 S1 119.76(13) . . ?
C7 Re1 S3 93.2(3) . . ?
N1 Re1 S3 84.5(2) . . ?
S2 Re1 S3 120.03(14) . . ?
S1 Re1 S3 118.30(12) . . ?
C2 S1 Re1 102.2(4) . . ?
C4 S2 Re1 102.5(4) . . ?
C6 S3 Re1 103.3(4) . . ?
C5 N1 C1 110.5(9) . . ?
C5 N1 C3 107.2(9) . . ?
C1 N1 C3 109.5(9) . . ?
C5 N1 Re1 110.9(7) . . ?
C1 N1 Re1 109.8(6) . . ?
C3 N1 Re1 109.0(6) . . ?
C7 N2 C8 152.4(11) . . ?
C10 N3 C11 126.5(8) . . ?
C10 N3 H3A 116.7 . . ?
C11 N3 H3A 116.7 . . ?
C17 N4 C14 115.4(8) . . ?
C18 N5 C17 116.8(8) . . ?
C18 N6 C19 126.7(8) . . ?
C18 N6 H6A 116.6 . . ?
C19 N6 H6A 116.6 . . ?
N1 C1 C2 115.1(10) . . ?
N1 C1 H1A 108.5 . . ?
C2 C1 H1A 108.5 . . ?
N1 C1 H1B 108.5 . . ?
C2 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
C1 C2 S1 111.8(8) . . ?
C1 C2 H2B 109.3 . . ?
S1 C2 H2B 109.3 . . ?
C1 C2 H2C 109.3 . . ?
S1 C2 H2C 109.3 . . ?
H2B C2 H2C 107.9 . . ?
C4 C3 N1 114.4(10) . . ?
C4 C3 H3B 108.7 . . ?
N1 C3 H3B 108.7 . . ?
C4 C3 H3C 108.7 . . ?
N1 C3 H3C 108.7 . . ?
H3B C3 H3C 107.6 . . ?
C3 C4 S2 111.7(8) . . ?
C3 C4 H4B 109.3 . . ?
S2 C4 H4B 109.3 . . ?
C3 C4 H4C 109.3 . . ?
S2 C4 H4C 109.3 . . ?
H4B C4 H4C 107.9 . . ?
N1 C5 C6 112.5(9) . . ?
N1 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
N1 C5 H5C 109.1 . . ?
C6 C5 H5C 109.1 . . ?
H5B C5 H5C 107.8 . . ?
C5 C6 S3 110.2(8) . . ?
C5 C6 H6B 109.6 . . ?
S3 C6 H6B 109.6 . . ?
C5 C6 H6C 109.6 . . ?
S3 C6 H6C 109.6 . . ?
H6B C6 H6C 108.1 . . ?
N2 C7 Re1 176.7(10) . . ?
N2 C8 C9 112.6(9) . . ?
N2 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N2 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C8 112.6(8) . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
O1 C10 N3 121.2(9) . . ?
O1 C10 C9 124.1(10) . . ?
N3 C10 C9 114.7(8) . . ?
C16 C11 C12 120.4(9) . . ?
C16 C11 N3 121.8(9) . . ?
C12 C11 N3 117.7(8) . . ?
C13 C12 C11 119.2(8) . . ?
C13 C12 H12A 120.4 . . ?
C11 C12 H12A 120.4 . . ?
C12 C13 C14 122.6(9) . . ?
C12 C13 H13A 118.7 . . ?
C14 C13 H13A 118.7 . . ?
C13 C14 N4 120.6(9) . . ?
C13 C14 C15 117.8(9) . . ?
N4 C14 C15 121.6(8) . . ?
C14 C15 C16 119.5(8) . . ?
C14 C15 C18 115.8(9) . . ?
C16 C15 C18 124.7(8) . . ?
C11 C16 C15 120.5(9) . . ?
C11 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
N4 C17 N5 128.5(10) . . ?
N4 C17 H17A 115.8 . . ?
N5 C17 H17A 115.8 . . ?
N5 C18 N6 120.3(8) . . ?
N5 C18 C15 121.5(9) . . ?
N6 C18 C15 118.2(9) . . ?
C20 C19 C24 119.0(9) . . ?
C20 C19 N6 123.4(9) . . ?
C24 C19 N6 117.4(9) . . ?
C19 C20 C21 120.7(10) . . ?
C19 C20 H20A 119.7 . . ?
C21 C20 H20A 119.7 . . ?
C22 C21 C20 121.4(11) . . ?
C22 C21 H21A 119.3 . . ?
C20 C21 H21A 119.3 . . ?
C21 C22 C23 118.3(10) . . ?
C21 C22 H22A 120.8 . . ?
C23 C22 H22A 120.8 . . ?
C22 C23 C24 121.8(10) . . ?
C22 C23 Br1 119.6(8) . . ?
C24 C23 Br1 118.6(8) . . ?
C19 C24 C23 118.8(9) . . ?
C19 C24 H24A 120.6 . . ?
C23 C24 H24A 120.6 . . ?
H4D O4 H4E 93(7) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.268
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.162


# Attachment 'Re-complex_9.cif'

data_repzb_s
_database_code_depnum_ccdc_archive 'CCDC 676394'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'4(C12 H14 N3 O5 Re), H2 O, 0.5(H2 O), 0.5(H2 O)'
_chemical_formula_sum            'C48 H60 N12 O22 Re4'
_chemical_formula_weight         1901.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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                   11.3584(15)
_cell_length_b                   14.756(2)
_cell_length_c                   19.845(2)
_cell_angle_alpha                88.445(11)
_cell_angle_beta                 88.414(10)
_cell_angle_gamma                76.384(12)
_cell_volume                     3230.7(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      8
_cell_measurement_theta_max      12

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1816
_exptl_absorpt_coefficient_mu    7.549
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.1273
_exptl_absorpt_correction_T_max  0.4212
_exptl_absorpt_process_details   'psi-scan (North et al.,1968)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       \w-2\q
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         5
_diffrn_standards_interval_count 500
_diffrn_standards_interval_time  5200
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12870
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.58
_diffrn_reflns_theta_max         25.68
_reflns_number_total             12217
_reflns_number_gt                8694
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD4 Software (Enraf-Nonius,1994) '
_computing_cell_refinement       'CAD4 Software (Enraf-Nonius,1994) '
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep3( Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

_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.

Restraints on displacement parameters were applied for C43, C44, C45, C46
atoms of one and O atoms of desorder water molecules using ISOR instructions
in SHELXL97 (Sheldrick,1997).

The existence of voids in the lattice indicate the presence of disorder
solvent (squeeze instruction was applied), however, due to absence of
residual density it was not possible identify and modulate the disorder
solvent molecules.
;

_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^)+(0.0660P)^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         12217
_refine_ls_number_parameters     783
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1105
_refine_ls_wR_factor_gt          0.1009
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.971
_refine_ls_shift/su_max          0.002
_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
Re1 Re 0.00850(3) 0.98023(2) 0.781271(19) 0.03469(10) Uani 1 1 d . . .
Re2 Re 0.17438(3) 0.46518(2) 0.821097(19) 0.03576(10) Uani 1 1 d . . .
Re3 Re 0.59608(3) 0.78456(3) 0.839433(19) 0.03702(10) Uani 1 1 d . . .
Re4 Re 0.65740(4) 0.24264(3) 0.59848(2) 0.05655(13) Uani 1 1 d . . .
O33 O 0.7717(5) 0.7811(4) 0.7943(3) 0.0399(15) Uani 1 1 d . . .
C30 C 0.4442(9) 0.7756(7) 0.8760(6) 0.052(3) Uani 1 1 d . . .
C28 C 0.4969(9) 0.3412(7) 0.9363(5) 0.051(3) Uani 1 1 d . . .
H28 H 0.5523 0.3399 0.9701 0.061 Uiso 1 1 calc R . .
O42 O 0.6481(8) 0.1920(7) 0.7473(4) 0.084(3) Uani 1 1 d . . .
O2 O -0.2505(7) 1.0024(6) 0.8355(5) 0.079(3) Uani 1 1 d . . .
C8 C 0.1246(8) 0.8917(6) 0.9836(5) 0.040(2) Uani 1 1 d . . .
O30 O 0.3531(7) 0.7662(6) 0.8993(5) 0.079(3) Uani 1 1 d . . .
N3 N 0.0589(6) 0.8251(5) 0.7782(4) 0.0370(17) Uani 1 1 d . . .
H3 H -0.0028 0.8094 0.7566 0.044 Uiso 1 1 calc R . .
O31 O 0.6442(8) 0.8722(6) 0.9694(4) 0.082(3) Uani 1 1 d . . .
C11 C 0.1260(10) 0.8234(7) 1.0386(5) 0.060(3) Uani 1 1 d . . .
H11A H 0.0767 0.7816 1.0273 0.090 Uiso 1 1 calc R . .
H11B H 0.0944 0.8552 1.0792 0.090 Uiso 1 1 calc R . .
H11C H 0.2076 0.7886 1.0455 0.090 Uiso 1 1 calc R . .
O23 O 0.2789(6) 0.5502(4) 0.7689(3) 0.0432(15) Uani 1 1 d . . .
O1 O -0.0870(8) 0.9965(6) 0.6386(4) 0.082(3) Uani 1 1 d . . .
N8 N 0.6539(7) 0.5658(5) 0.8291(4) 0.0432(19) Uani 1 1 d . . .
C1 C -0.0514(9) 0.9900(7) 0.6919(5) 0.049(2) Uani 1 1 d . . .
O20 O 0.0440(7) 0.3264(5) 0.8882(4) 0.065(2) Uani 1 1 d . . .
C6 C 0.0718(9) 0.7694(6) 0.8417(5) 0.047(2) Uani 1 1 d . . .
H6A H 0.1572 0.7493 0.8517 0.057 Uiso 1 1 calc R . .
H6B H 0.0419 0.7139 0.8350 0.057 Uiso 1 1 calc R . .
N12 N 0.6564(12) 0.2783(9) 0.4909(5) 0.092(4) Uani 1 1 d . . .
H12 H 0.6552 0.3398 0.4849 0.111 Uiso 1 1 calc R . .
O43 O 0.4711(8) 0.2625(6) 0.5771(5) 0.078(3) Uani 1 1 d D . .
C20 C 0.0937(9) 0.3797(6) 0.8623(5) 0.044(2) Uani 1 1 d . . .
N4 N 0.3482(6) 0.3934(5) 0.8634(3) 0.0332(16) Uani 1 1 d . . .
N1 N 0.0869(6) 0.9584(5) 0.8813(4) 0.0373(17) Uani 1 1 d . . .
O4 O 0.1940(5) 0.9504(4) 0.7486(3) 0.0445(16) Uani 1 1 d . . .
C5 C 0.1652(9) 0.7971(7) 0.7326(5) 0.049(2) Uani 1 1 d . . .
H5A H 0.1378 0.7880 0.6879 0.058 Uiso 1 1 calc R . .
H5B H 0.2147 0.7380 0.7485 0.058 Uiso 1 1 calc R . .
C21 C 0.0266(9) 0.5239(7) 0.7794(5) 0.049(3) Uani 1 1 d . . .
N6 N 0.2450(7) 0.3845(5) 0.7307(4) 0.0386(17) Uani 1 1 d . . .
H6 H 0.1856 0.3576 0.7170 0.046 Uiso 1 1 calc R . .
N9 N 0.5850(6) 0.7410(5) 0.7341(4) 0.0358(17) Uani 1 1 d . . .
H90 H 0.5079 0.7662 0.7209 0.043 Uiso 1 1 calc R . .
C23 C 0.3040(9) 0.5343(7) 0.7061(5) 0.049(2) Uani 1 1 d . . .
C22 C 0.1244(8) 0.5398(6) 0.8963(5) 0.042(2) Uani 1 1 d . . .
N7 N 0.6750(6) 0.6373(5) 0.8646(4) 0.0379(17) Uani 1 1 d . . .
O41 O 0.6319(13) 0.4420(7) 0.6424(5) 0.122(4) Uani 1 1 d . . .
C42 C 0.6500(10) 0.2102(8) 0.6908(6) 0.060(3) Uani 1 1 d . . .
O21 O -0.0665(7) 0.5599(6) 0.7560(5) 0.081(3) Uani 1 1 d . . .
C35 C 0.6115(9) 0.6397(6) 0.7178(5) 0.044(2) Uani 1 1 d . . .
H35A H 0.5723 0.6320 0.6762 0.053 Uiso 1 1 calc R . .
H35B H 0.6981 0.6164 0.7110 0.053 Uiso 1 1 calc R . .
O5 O 0.3455(6) 0.8457(5) 0.7027(4) 0.0571(19) Uani 1 1 d . . .
O24 O 0.3567(7) 0.5808(5) 0.6704(4) 0.068(2) Uani 1 1 d . . .
C41 C 0.6399(14) 0.3683(10) 0.6252(6) 0.080(4) Uani 1 1 d . . .
C491 C 0.5286(13) 0.0456(9) 0.6355(8) 0.088(4) Uani 1 1 d . . .
H49A H 0.5228 0.1047 0.6561 0.132 Uiso 1 1 calc R . .
H49B H 0.5576 -0.0038 0.6677 0.132 Uiso 1 1 calc R . .
H49C H 0.4501 0.0420 0.6208 0.132 Uiso 1 1 calc R . .
C24 C 0.2621(10) 0.4522(7) 0.6774(5) 0.053(3) Uani 1 1 d . . .
H24A H 0.1863 0.4755 0.6544 0.064 Uiso 1 1 calc R . .
H24B H 0.3217 0.4211 0.6445 0.064 Uiso 1 1 calc R . .
N2 N 0.0689(6) 0.8907(4) 0.9248(4) 0.0345(16) Uani 1 1 d . . .
O40 O 0.9303(9) 0.2137(8) 0.6180(6) 0.100(3) Uani 1 1 d . . .
C4 C 0.2428(8) 0.8691(7) 0.7277(5) 0.040(2) Uani 1 1 d . . .
C2 C -0.1519(9) 0.9946(6) 0.8142(6) 0.049(2) Uani 1 1 d . . .
O22 O 0.0951(7) 0.5864(5) 0.9443(4) 0.061(2) Uani 1 1 d . . .
C32 C 0.5240(9) 0.9107(7) 0.8157(5) 0.049(2) Uani 1 1 d . . .
C49 C 0.6133(12) 0.0363(8) 0.5773(7) 0.069(3) Uani 1 1 d . . .
O32 O 0.4780(7) 0.9880(5) 0.8022(5) 0.072(2) Uani 1 1 d . . .
C31 C 0.6276(10) 0.8357(8) 0.9225(6) 0.056(3) Uani 1 1 d . . .
C34 C 0.6649(8) 0.7872(7) 0.6922(5) 0.042(2) Uani 1 1 d . . .
H34A H 0.6236 0.8513 0.6823 0.050 Uiso 1 1 calc R . .
H34B H 0.6851 0.7552 0.6498 0.050 Uiso 1 1 calc R . .
C29 C 0.4169(8) 0.4206(6) 0.9104(5) 0.042(2) Uani 1 1 d . . .
N5 N 0.3879(7) 0.2995(5) 0.8600(4) 0.0381(17) Uani 1 1 d . . .
C39 C 0.7552(8) 0.5969(8) 0.9121(5) 0.048(2) Uani 1 1 d . . .
C7 C 0.0062(8) 0.8196(6) 0.9014(5) 0.042(2) Uani 1 1 d . . .
H7A H -0.0761 0.8499 0.8893 0.051 Uiso 1 1 calc R . .
H7B H 0.0023 0.7750 0.9377 0.051 Uiso 1 1 calc R . .
C291 C 0.4000(9) 0.5216(6) 0.9274(5) 0.047(2) Uani 1 1 d . . .
H29A H 0.3381 0.5590 0.8998 0.070 Uiso 1 1 calc R . .
H29B H 0.4747 0.5402 0.9192 0.070 Uiso 1 1 calc R . .
H29C H 0.3763 0.5300 0.9740 0.070 Uiso 1 1 calc R . .
C9 C 0.1816(9) 0.9639(6) 0.9773(5) 0.046(2) Uani 1 1 d . . .
H9 H 0.2282 0.9828 1.0095 0.056 Uiso 1 1 calc R . .
C38 C 0.7848(9) 0.5012(7) 0.9034(5) 0.050(3) Uani 1 1 d . . .
H38 H 0.8390 0.4574 0.9290 0.061 Uiso 1 1 calc R . .
C47 C 0.7298(14) -0.0100(8) 0.4866(8) 0.078(4) Uani 1 1 d . . .
C10 C 0.1564(8) 1.0029(6) 0.9144(5) 0.042(2) Uani 1 1 d . . .
C27 C 0.4791(9) 0.2658(7) 0.9031(5) 0.047(2) Uani 1 1 d . . .
C12 C 0.2047(9) 1.0819(7) 0.8827(5) 0.052(3) Uani 1 1 d . . .
H12A H 0.1726 1.0960 0.8384 0.078 Uiso 1 1 calc R . .
H12B H 0.2915 1.0636 0.8796 0.078 Uiso 1 1 calc R . .
H12C H 0.1805 1.1362 0.9100 0.078 Uiso 1 1 calc R . .
C46 C 0.8125(16) 0.1316(12) 0.4704(9) 0.113(5) Uani 1 1 d U . .
H46A H 0.8553 0.0981 0.4322 0.136 Uiso 1 1 calc R . .
H46B H 0.8728 0.1405 0.5016 0.136 Uiso 1 1 calc R . .
C26 C 0.3524(9) 0.2545(6) 0.8026(5) 0.046(2) Uani 1 1 d . . .
H26A H 0.2713 0.2456 0.8107 0.056 Uiso 1 1 calc R . .
H26B H 0.4067 0.1934 0.7978 0.056 Uiso 1 1 calc R . .
C391 C 0.8008(10) 0.6511(9) 0.9626(5) 0.065(3) Uani 1 1 d . . .
H39A H 0.7651 0.7164 0.9557 0.097 Uiso 1 1 calc R . .
H39B H 0.8873 0.6402 0.9580 0.097 Uiso 1 1 calc R . .
H39C H 0.7796 0.6321 1.0071 0.097 Uiso 1 1 calc R . .
C40 C 0.8275(13) 0.2244(8) 0.6108(6) 0.069(3) Uani 1 1 d . . .
N10 N 0.6674(8) 0.1036(6) 0.5591(5) 0.062(2) Uani 1 1 d . . .
C37 C 0.7225(9) 0.4834(7) 0.8524(5) 0.048(2) Uani 1 1 d . . .
N11 N 0.7388(9) 0.0731(7) 0.5040(5) 0.072(3) Uani 1 1 d . . .
C25 C 0.3548(9) 0.3100(7) 0.7376(5) 0.049(2) Uani 1 1 d . . .
H25A H 0.4250 0.3369 0.7366 0.058 Uiso 1 1 calc R . .
H25B H 0.3624 0.2686 0.6997 0.058 Uiso 1 1 calc R . .
C36 C 0.5681(9) 0.5845(7) 0.7727(5) 0.047(2) Uani 1 1 d . . .
H36A H 0.4893 0.6184 0.7892 0.056 Uiso 1 1 calc R . .
H36B H 0.5593 0.5258 0.7552 0.056 Uiso 1 1 calc R . .
C371 C 0.7207(12) 0.3924(7) 0.8157(7) 0.079(4) Uani 1 1 d . . .
H37A H 0.6643 0.4063 0.7796 0.119 Uiso 1 1 calc R . .
H37B H 0.6966 0.3491 0.8470 0.119 Uiso 1 1 calc R . .
H37C H 0.8002 0.3654 0.7978 0.119 Uiso 1 1 calc R . .
C48 C 0.6529(16) -0.0357(10) 0.5325(8) 0.098(5) Uani 1 1 d . . .
H48 H 0.6302 -0.0923 0.5339 0.118 Uiso 1 1 calc R . .
C271 C 0.5429(10) 0.1671(7) 0.9097(6) 0.058(3) Uani 1 1 d . . .
H27A H 0.5099 0.1310 0.8790 0.087 Uiso 1 1 calc R . .
H27B H 0.5330 0.1453 0.9550 0.087 Uiso 1 1 calc R . .
H27C H 0.6275 0.1607 0.8995 0.087 Uiso 1 1 calc R . .
O34 O 0.8736(6) 0.7856(5) 0.6976(4) 0.0582(19) Uani 1 1 d . . .
C33 C 0.7795(8) 0.7843(6) 0.7306(5) 0.041(2) Uani 1 1 d . . .
O3 O -0.0458(9) 1.1930(5) 0.7778(5) 0.085(3) Uani 1 1 d . . .
C3 C -0.0211(10) 1.1142(7) 0.7794(5) 0.053(3) Uani 1 1 d . . .
C45 C 0.7442(19) 0.2241(14) 0.4462(9) 0.129(6) Uani 1 1 d U . .
H45A H 0.8024 0.2606 0.4336 0.155 Uiso 1 1 calc R . .
H45B H 0.7033 0.2152 0.4056 0.155 Uiso 1 1 calc R . .
C471 C 0.7984(16) -0.0601(11) 0.4297(9) 0.122(6) Uani 1 1 d . . .
H47A H 0.7784 -0.1194 0.4259 0.183 Uiso 1 1 calc R . .
H47B H 0.8836 -0.0695 0.4372 0.183 Uiso 1 1 calc R . .
H47C H 0.7781 -0.0241 0.3889 0.183 Uiso 1 1 calc R . .
O44 O 0.3296(16) 0.2768(12) 0.4977(9) 0.173(6) Uani 1 1 d DU . .
C44 C 0.438(2) 0.2758(19) 0.5164(10) 0.170(9) Uani 1 1 d DU . .
C43 C 0.548(2) 0.2583(18) 0.4619(12) 0.168(9) Uani 1 1 d U . .
H43A H 0.5654 0.1940 0.4477 0.201 Uiso 1 1 calc R . .
H43B H 0.5244 0.2983 0.4225 0.201 Uiso 1 1 calc R . .
O1W O 0.6153(14) 0.4581(11) 0.4684(8) 0.177(6) Uani 1 1 d U . .
H11W H 0.6157 0.4716 0.4265 0.212 Uiso 1 1 d R . .
H21W H 0.6328 0.5026 0.4892 0.212 Uiso 1 1 d R . .
O2W O 0.071(3) 0.322(2) 0.6613(13) 0.200(13) Uani 0.50 1 d PDU . .
H12W H 0.0110 0.3049 0.6792 0.240 Uiso 0.50 1 d PR . .
H22W H 0.0539 0.3813 0.6595 0.240 Uiso 0.50 1 d PR . .
O3W O 0.135(3) 0.3194(19) 0.5548(13) 0.1649(9) Uani 0.50 1 d PDU . .
H13W H 0.0881 0.3052 0.5267 0.198 Uiso 0.50 1 d PR . .
H23W H 0.2063 0.3074 0.5371 0.198 Uiso 0.50 1 d PR . .

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
Re1 0.03408(19) 0.02871(18) 0.0407(2) -0.00123(15) -0.00342(15) -0.00591(14)
Re2 0.03559(19) 0.03087(18) 0.0407(2) 0.00082(15) 0.00011(15) -0.00777(15)
Re3 0.03149(19) 0.0404(2) 0.0409(2) -0.00906(16) -0.00233(15) -0.01078(15)
Re4 0.0740(3) 0.0550(3) 0.0361(2) -0.00244(19) 0.0048(2) -0.0065(2)
O33 0.028(3) 0.046(4) 0.050(4) -0.007(3) -0.004(3) -0.016(3)
C30 0.044(6) 0.050(6) 0.060(7) -0.023(5) 0.014(5) -0.009(5)
C28 0.046(6) 0.058(6) 0.049(6) 0.004(5) -0.009(5) -0.011(5)
O42 0.092(7) 0.115(7) 0.042(5) 0.012(5) 0.003(4) -0.017(6)
O2 0.039(4) 0.066(5) 0.129(8) -0.019(5) 0.024(5) -0.004(4)
C8 0.040(5) 0.038(5) 0.040(5) 0.000(4) 0.001(4) -0.004(4)
O30 0.042(4) 0.089(6) 0.105(7) -0.027(5) 0.028(4) -0.015(4)
N3 0.029(4) 0.037(4) 0.044(5) -0.006(3) -0.002(3) -0.005(3)
O31 0.106(7) 0.100(7) 0.059(5) -0.034(5) 0.004(5) -0.059(6)
C11 0.070(7) 0.055(6) 0.052(7) 0.016(5) 0.003(6) -0.014(6)
O23 0.050(4) 0.040(3) 0.044(4) 0.001(3) -0.002(3) -0.021(3)
O1 0.097(7) 0.082(6) 0.063(6) 0.001(5) -0.033(5) -0.008(5)
N8 0.041(4) 0.036(4) 0.055(5) -0.003(4) 0.003(4) -0.014(3)
C1 0.058(6) 0.044(6) 0.042(6) 0.001(5) -0.011(5) -0.005(5)
O20 0.069(5) 0.044(4) 0.087(6) 0.008(4) 0.010(4) -0.025(4)
C6 0.060(6) 0.026(4) 0.054(6) 0.002(4) -0.012(5) -0.006(4)
N12 0.114(10) 0.117(10) 0.044(6) 0.003(6) 0.015(6) -0.025(8)
O43 0.078(6) 0.074(6) 0.069(6) -0.002(5) -0.009(5) 0.012(5)
C20 0.050(6) 0.035(5) 0.048(6) 0.008(4) -0.007(5) -0.011(4)
N4 0.037(4) 0.031(4) 0.032(4) 0.000(3) -0.001(3) -0.009(3)
N1 0.041(4) 0.027(4) 0.044(5) 0.002(3) -0.006(3) -0.008(3)
O4 0.039(3) 0.044(4) 0.053(4) -0.006(3) 0.005(3) -0.016(3)
C5 0.050(6) 0.048(6) 0.049(6) -0.018(5) 0.010(5) -0.014(5)
C21 0.042(6) 0.049(6) 0.051(6) 0.013(5) 0.006(5) -0.002(5)
N6 0.046(4) 0.039(4) 0.037(4) -0.009(3) -0.007(3) -0.022(4)
N9 0.027(4) 0.036(4) 0.045(5) -0.003(3) -0.001(3) -0.010(3)
C23 0.049(6) 0.053(6) 0.045(6) 0.012(5) 0.000(5) -0.013(5)
C22 0.043(5) 0.038(5) 0.043(6) 0.008(4) 0.008(4) -0.006(4)
N7 0.033(4) 0.041(4) 0.039(4) -0.002(3) -0.005(3) -0.006(3)
O41 0.197(13) 0.069(6) 0.093(8) -0.030(6) 0.005(8) -0.018(7)
C42 0.066(7) 0.070(7) 0.040(7) -0.001(5) 0.009(5) -0.007(6)
O21 0.053(5) 0.092(6) 0.088(7) 0.020(5) -0.013(4) 0.002(5)
C35 0.043(5) 0.044(5) 0.044(6) -0.013(4) -0.017(4) -0.003(4)
O5 0.035(4) 0.073(5) 0.059(5) -0.010(4) 0.003(3) -0.005(3)
O24 0.088(6) 0.065(5) 0.058(5) 0.017(4) 0.012(4) -0.036(4)
C41 0.117(11) 0.072(9) 0.041(7) 0.003(6) -0.002(7) -0.004(8)
C491 0.100(11) 0.071(9) 0.100(11) 0.012(8) 0.015(9) -0.037(8)
C24 0.067(7) 0.054(6) 0.045(6) -0.004(5) -0.004(5) -0.026(5)
N2 0.043(4) 0.024(3) 0.039(4) -0.001(3) 0.003(3) -0.013(3)
O40 0.067(6) 0.122(9) 0.116(9) -0.025(7) 0.002(6) -0.030(6)
C4 0.031(5) 0.051(6) 0.036(5) -0.002(4) 0.001(4) -0.007(4)
C2 0.047(6) 0.030(5) 0.065(7) -0.007(5) 0.005(5) -0.002(4)
O22 0.066(5) 0.054(4) 0.052(5) -0.006(4) 0.005(4) 0.004(4)
C32 0.043(5) 0.055(6) 0.052(6) -0.020(5) 0.006(5) -0.015(5)
C49 0.072(8) 0.041(6) 0.092(10) 0.009(6) -0.007(7) -0.010(6)
O32 0.071(5) 0.044(4) 0.095(7) -0.013(4) 0.005(5) 0.000(4)
C31 0.057(6) 0.069(7) 0.050(7) -0.024(6) 0.006(5) -0.030(6)
C34 0.037(5) 0.045(5) 0.044(6) 0.000(4) -0.007(4) -0.010(4)
C29 0.040(5) 0.046(5) 0.039(5) 0.003(4) 0.003(4) -0.011(4)
N5 0.041(4) 0.024(3) 0.048(5) -0.004(3) 0.005(4) -0.006(3)
C39 0.034(5) 0.072(7) 0.040(6) 0.000(5) 0.004(4) -0.016(5)
C7 0.038(5) 0.041(5) 0.052(6) 0.005(4) -0.005(4) -0.019(4)
C291 0.055(6) 0.044(5) 0.045(6) -0.015(4) 0.008(5) -0.017(5)
C9 0.052(6) 0.040(5) 0.049(6) -0.010(4) -0.007(5) -0.013(5)
C38 0.045(6) 0.054(6) 0.048(6) 0.006(5) -0.004(5) -0.003(5)
C47 0.102(11) 0.041(6) 0.086(10) -0.009(6) -0.002(8) -0.003(7)
C10 0.045(5) 0.027(4) 0.051(6) -0.004(4) 0.000(5) -0.004(4)
C27 0.042(5) 0.049(6) 0.040(6) 0.006(5) 0.011(4) 0.008(5)
C12 0.057(6) 0.045(6) 0.061(7) -0.004(5) -0.002(5) -0.026(5)
C46 0.117(9) 0.115(9) 0.114(9) -0.038(7) 0.026(7) -0.038(7)
C26 0.052(6) 0.033(5) 0.057(6) -0.012(4) 0.005(5) -0.014(4)
C391 0.056(7) 0.098(9) 0.047(7) 0.016(6) -0.020(5) -0.031(6)
C40 0.083(9) 0.061(7) 0.055(8) 0.000(6) 0.019(7) -0.003(7)
N10 0.063(6) 0.055(6) 0.065(6) -0.006(5) -0.003(5) -0.005(5)
C37 0.042(5) 0.058(6) 0.041(6) 0.008(5) 0.018(5) -0.009(5)
N11 0.072(7) 0.069(7) 0.070(7) -0.016(5) 0.016(6) -0.009(5)
C25 0.064(7) 0.046(6) 0.040(6) -0.013(4) 0.004(5) -0.021(5)
C36 0.048(6) 0.044(5) 0.056(6) 0.003(5) -0.009(5) -0.025(5)
C371 0.092(9) 0.040(6) 0.093(10) 0.011(6) 0.005(8) 0.008(6)
C48 0.132(14) 0.059(8) 0.097(12) 0.003(8) -0.004(11) -0.009(9)
C271 0.056(6) 0.047(6) 0.062(7) 0.006(5) 0.001(5) 0.006(5)
O34 0.057(4) 0.078(5) 0.053(5) -0.008(4) 0.005(4) -0.042(4)
C33 0.044(5) 0.043(5) 0.039(6) 0.004(4) 0.000(4) -0.016(4)
O3 0.133(8) 0.036(4) 0.082(6) 0.002(4) -0.030(6) -0.008(5)
C3 0.072(7) 0.041(6) 0.050(7) 0.006(5) -0.007(5) -0.020(5)
C45 0.158(10) 0.134(10) 0.093(9) -0.001(8) 0.018(8) -0.030(8)
C471 0.133(15) 0.095(12) 0.127(15) -0.054(11) 0.028(12) 0.000(11)
O44 0.172(6) 0.174(6) 0.172(6) -0.004(2) -0.006(2) -0.041(2)
C44 0.149(12) 0.189(12) 0.170(12) -0.012(9) -0.006(9) -0.037(9)
C43 0.175(12) 0.175(12) 0.150(12) 0.020(9) -0.005(9) -0.038(9)
O1W 0.177(6) 0.177(6) 0.176(6) -0.0035(10) -0.0038(10) -0.0415(17)
O2W 0.200(13) 0.200(13) 0.200(13) -0.0042(11) -0.0048(11) -0.047(3)
O3W 0.1648(15) 0.1649(15) 0.165 -0.0036(10) -0.0035(10) -0.0388(10)

_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
Re1 C2 1.885(11) . ?
Re1 C1 1.907(10) . ?
Re1 C3 1.926(10) . ?
Re1 O4 2.135(6) . ?
Re1 N1 2.182(7) . ?
Re1 N3 2.226(7) . ?
Re2 C22 1.874(10) . ?
Re2 C20 1.884(10) . ?
Re2 C21 1.900(10) . ?
Re2 O23 2.149(6) . ?
Re2 N4 2.187(7) . ?
Re2 N6 2.205(7) . ?
Re3 C30 1.885(11) . ?
Re3 C32 1.901(11) . ?
Re3 C31 1.908(10) . ?
Re3 O33 2.154(6) . ?
Re3 N7 2.196(7) . ?
Re3 N9 2.220(7) . ?
Re4 C42 1.885(11) . ?
Re4 C41 1.906(15) . ?
Re4 C40 1.908(15) . ?
Re4 O43 2.120(9) . ?
Re4 N12 2.185(10) . ?
Re4 N10 2.192(9) . ?
O33 C33 1.264(11) . ?
C30 O30 1.158(12) . ?
C28 C27 1.366(14) . ?
C28 C29 1.398(13) . ?
O42 C42 1.148(12) . ?
O2 C2 1.166(12) . ?
C8 N2 1.345(11) . ?
C8 C9 1.373(13) . ?
C8 C11 1.463(13) . ?
N3 C5 1.474(11) . ?
N3 C6 1.478(11) . ?
O31 C31 1.131(12) . ?
O23 C23 1.286(12) . ?
O1 C1 1.135(12) . ?
N8 N7 1.355(10) . ?
N8 C37 1.359(12) . ?
N8 C36 1.481(12) . ?
O20 C20 1.172(11) . ?
C6 C7 1.499(13) . ?
N12 C45 1.426(19) . ?
N12 C43 1.47(2) . ?
O43 C44 1.267(16) . ?
N4 N5 1.355(9) . ?
N4 C29 1.359(11) . ?
N1 C10 1.336(11) . ?
N1 N2 1.351(9) . ?
O4 C4 1.272(10) . ?
C5 C4 1.531(13) . ?
C21 O21 1.168(11) . ?
N6 C25 1.463(12) . ?
N6 C24 1.476(12) . ?
N9 C34 1.482(11) . ?
N9 C35 1.496(11) . ?
C23 O24 1.213(12) . ?
C23 C24 1.531(14) . ?
C22 O22 1.183(11) . ?
N7 C39 1.354(12) . ?
O41 C41 1.131(15) . ?
C35 C36 1.484(13) . ?
O5 C4 1.230(10) . ?
C491 C49 1.472(18) . ?
N2 C7 1.489(11) . ?
O40 C40 1.153(15) . ?
C32 O32 1.164(12) . ?
C49 N10 1.323(15) . ?
C49 C48 1.387(18) . ?
C34 C33 1.519(12) . ?
C29 C291 1.504(12) . ?
N5 C27 1.355(12) . ?
N5 C26 1.447(12) . ?
C39 C38 1.388(14) . ?
C39 C391 1.477(15) . ?
C9 C10 1.368(13) . ?
C38 C37 1.318(14) . ?
C47 N11 1.310(15) . ?
C47 C48 1.35(2) . ?
C47 C471 1.468(19) . ?
C10 C12 1.516(13) . ?
C27 C271 1.469(13) . ?
C46 N11 1.473(19) . ?
C46 C45 1.48(2) . ?
C26 C25 1.511(13) . ?
N10 N11 1.364(13) . ?
C37 C371 1.549(15) . ?
O34 C33 1.242(11) . ?
O3 C3 1.129(11) . ?
O44 C44 1.292(16) . ?
C44 C43 1.61(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Re1 C1 88.7(5) . . ?
C2 Re1 C3 87.3(4) . . ?
C1 Re1 C3 87.3(4) . . ?
C2 Re1 O4 174.3(3) . . ?
C1 Re1 O4 93.9(4) . . ?
C3 Re1 O4 98.0(4) . . ?
C2 Re1 N1 94.0(4) . . ?
C1 Re1 N1 175.4(3) . . ?
C3 Re1 N1 96.6(4) . . ?
O4 Re1 N1 83.1(3) . . ?
C2 Re1 N3 98.0(3) . . ?
C1 Re1 N3 91.9(3) . . ?
C3 Re1 N3 174.6(4) . . ?
O4 Re1 N3 76.8(2) . . ?
N1 Re1 N3 84.0(3) . . ?
C22 Re2 C20 86.7(4) . . ?
C22 Re2 C21 88.8(4) . . ?
C20 Re2 C21 88.2(4) . . ?
C22 Re2 O23 98.8(3) . . ?
C20 Re2 O23 173.8(3) . . ?
C21 Re2 O23 94.7(3) . . ?
C22 Re2 N4 94.6(3) . . ?
C20 Re2 N4 92.4(3) . . ?
C21 Re2 N4 176.6(4) . . ?
O23 Re2 N4 84.4(2) . . ?
C22 Re2 N6 175.0(3) . . ?
C20 Re2 N6 98.0(4) . . ?
C21 Re2 N6 92.9(4) . . ?
O23 Re2 N6 76.4(3) . . ?
N4 Re2 N6 83.7(3) . . ?
C30 Re3 C32 87.8(4) . . ?
C30 Re3 C31 88.4(5) . . ?
C32 Re3 C31 84.0(5) . . ?
C30 Re3 O33 174.4(3) . . ?
C32 Re3 O33 96.6(3) . . ?
C31 Re3 O33 95.4(4) . . ?
C30 Re3 N7 91.3(4) . . ?
C32 Re3 N7 178.0(3) . . ?
C31 Re3 N7 97.7(4) . . ?
O33 Re3 N7 84.2(3) . . ?
C30 Re3 N9 101.8(4) . . ?
C32 Re3 N9 91.2(3) . . ?
C31 Re3 N9 168.5(4) . . ?
O33 Re3 N9 74.7(2) . . ?
N7 Re3 N9 87.3(3) . . ?
C42 Re4 C41 87.5(5) . . ?
C42 Re4 C40 85.5(5) . . ?
C41 Re4 C40 87.8(6) . . ?
C42 Re4 O43 98.6(4) . . ?
C41 Re4 O43 93.5(5) . . ?
C40 Re4 O43 175.8(4) . . ?
C42 Re4 N12 176.8(5) . . ?
C41 Re4 N12 93.7(5) . . ?
C40 Re4 N12 97.5(5) . . ?
O43 Re4 N12 78.5(4) . . ?
C42 Re4 N10 97.2(5) . . ?
C41 Re4 N10 174.4(4) . . ?
C40 Re4 N10 95.6(4) . . ?
O43 Re4 N10 82.8(3) . . ?
N12 Re4 N10 81.5(4) . . ?
C33 O33 Re3 117.4(6) . . ?
O30 C30 Re3 177.0(10) . . ?
C27 C28 C29 107.8(9) . . ?
N2 C8 C9 105.4(8) . . ?
N2 C8 C11 124.3(9) . . ?
C9 C8 C11 130.2(10) . . ?
C5 N3 C6 112.3(7) . . ?
C5 N3 Re1 108.2(6) . . ?
C6 N3 Re1 119.9(5) . . ?
C23 O23 Re2 117.4(6) . . ?
N7 N8 C37 110.2(8) . . ?
N7 N8 C36 120.3(7) . . ?
C37 N8 C36 129.5(8) . . ?
O1 C1 Re1 179.5(10) . . ?
N3 C6 C7 114.6(7) . . ?
C45 N12 C43 97.9(15) . . ?
C45 N12 Re4 120.1(11) . . ?
C43 N12 Re4 108.5(12) . . ?
C44 O43 Re4 119.1(13) . . ?
O20 C20 Re2 179.6(9) . . ?
N5 N4 C29 105.9(7) . . ?
N5 N4 Re2 120.9(5) . . ?
C29 N4 Re2 130.8(6) . . ?
C10 N1 N2 104.6(7) . . ?
C10 N1 Re1 132.4(6) . . ?
N2 N1 Re1 123.0(5) . . ?
C4 O4 Re1 118.7(6) . . ?
N3 C5 C4 112.9(7) . . ?
O21 C21 Re2 177.4(9) . . ?
C25 N6 C24 110.6(8) . . ?
C25 N6 Re2 117.7(5) . . ?
C24 N6 Re2 107.0(6) . . ?
C34 N9 C35 109.4(7) . . ?
C34 N9 Re3 106.9(5) . . ?
C35 N9 Re3 120.2(5) . . ?
O24 C23 O23 123.5(10) . . ?
O24 C23 C24 120.7(10) . . ?
O23 C23 C24 115.9(9) . . ?
O22 C22 Re2 178.7(9) . . ?
C39 N7 N8 105.4(8) . . ?
C39 N7 Re3 131.3(7) . . ?
N8 N7 Re3 123.2(5) . . ?
O42 C42 Re4 177.9(12) . . ?
C36 C35 N9 111.4(8) . . ?
O41 C41 Re4 178.0(13) . . ?
N6 C24 C23 111.8(8) . . ?
C8 N2 N1 112.4(7) . . ?
C8 N2 C7 127.9(7) . . ?
N1 N2 C7 119.3(7) . . ?
O5 C4 O4 124.7(9) . . ?
O5 C4 C5 118.5(9) . . ?
O4 C4 C5 116.7(8) . . ?
O2 C2 Re1 178.8(10) . . ?
O32 C32 Re3 178.6(10) . . ?
N10 C49 C48 107.2(13) . . ?
N10 C49 C491 121.5(11) . . ?
C48 C49 C491 131.3(13) . . ?
O31 C31 Re3 174.9(11) . . ?
N9 C34 C33 108.7(7) . . ?
N4 C29 C28 108.4(8) . . ?
N4 C29 C291 121.3(8) . . ?
C28 C29 C291 130.3(9) . . ?
C27 N5 N4 111.9(8) . . ?
C27 N5 C26 128.4(8) . . ?
N4 N5 C26 117.5(7) . . ?
N7 C39 C38 108.8(9) . . ?
N7 C39 C391 122.7(10) . . ?
C38 C39 C391 128.4(10) . . ?
N2 C7 C6 110.8(8) . . ?
C10 C9 C8 106.8(9) . . ?
C37 C38 C39 107.7(9) . . ?
N11 C47 C48 105.7(13) . . ?
N11 C47 C471 123.1(15) . . ?
C48 C47 C471 131.1(14) . . ?
N1 C10 C9 110.8(8) . . ?
N1 C10 C12 122.6(9) . . ?
C9 C10 C12 126.4(9) . . ?
N5 C27 C28 105.9(8) . . ?
N5 C27 C271 124.7(10) . . ?
C28 C27 C271 129.4(10) . . ?
N11 C46 C45 115.2(15) . . ?
N5 C26 C25 112.7(8) . . ?
O40 C40 Re4 179.7(14) . . ?
C49 N10 N11 106.7(10) . . ?
C49 N10 Re4 132.8(9) . . ?
N11 N10 Re4 120.5(8) . . ?
C38 C37 N8 107.8(10) . . ?
C38 C37 C371 132.8(10) . . ?
N8 C37 C371 119.4(9) . . ?
C47 N11 N10 111.7(12) . . ?
C47 N11 C46 127.2(12) . . ?
N10 N11 C46 121.1(11) . . ?
N6 C25 C26 111.5(8) . . ?
N8 C36 C35 111.0(7) . . ?
C47 C48 C49 108.8(14) . . ?
O34 C33 O33 124.7(9) . . ?
O34 C33 C34 118.0(9) . . ?
O33 C33 C34 117.3(8) . . ?
O3 C3 Re1 175.8(11) . . ?
N12 C45 C46 118.0(15) . . ?
O43 C44 O44 123(2) . . ?
O43 C44 C43 114.2(18) . . ?
O44 C44 C43 119.8(19) . . ?
N12 C43 C44 110.4(18) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.601
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.175