# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_a616
_database_code_depnum_ccdc_archive 'CCDC 842922'
#TrackingRef '1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H31 F8.38 N10 O4.42 P1.40 Re1.61'
_chemical_formula_weight         1007.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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                   8.3330(5)
_cell_length_b                   9.7967(6)
_cell_length_c                   11.5140(7)
_cell_angle_alpha                112.1330(10)
_cell_angle_beta                 97.5260(10)
_cell_angle_gamma                101.0040(10)
_cell_volume                     833.13(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    6192
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      27.49

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             484.8
_exptl_absorpt_coefficient_mu    5.996
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.1193
_exptl_absorpt_correction_T_max  0.3193
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(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 detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10815
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3821
_reflns_number_gt                3672
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '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.

The anion which appears to be a mixture of PF6- and ReO4-. The disordered
anion pair were refined to a ratio of 0.70 PF6- to 0.30 ReO4-.
Restraints on geometries of the anions were applied because proximity of the
atoms led to poor L.S. convergence unless restraints were applied. H1O which
was half occupied was located from different map and refined with restraint
in bond length and and thermal parameters.
Details of the restraints applied :
DFIX 0.85 0.01 O1 H1O
SADI 0.004 F1 F3 F2 F4 F5 F6
EADP P1 Re2
SADI 0.005 F1 F2 F1 F4 F1 F5 F1 F6 F2 F3 F2 F5 F2 F6 F3 F4 F3 F5
DFIX 1.55 0.01 P1 F1 P1 F2 P1 F3 P1 F4 P1 F5 P1 F6
DFIX 1.7 0.02 Re2 O2 Re2 O3 Re2 O4 Re2 O5
SADI 0.005 O2 O3 O2 O4 O2 O5 O3 O4 O3 O5 O4 O5
SIZE 0.50 0.24 0.20
DELU 0.001 0.001 Re1 O1

For PLAT420_ALERT_2_B D-H Without Acceptor O1 - *H1O ... ? Response is:
There is a H bond to O of ReO4 or F of PF6 as listed below.
;

_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^)+(0.0269P)^2^+2.0377P] 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         3821
_refine_ls_number_parameters     267
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.0925
_refine_ls_wR_factor_gt          0.0915
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_restrained_S_all      1.250
_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 0.5000 0.5000 0.0000 0.04350(12) Uani 1 2 d SU . .
O1 O 0.7207(5) 0.5757(4) -0.0246(3) 0.0395(6) Uani 1 1 d DU . .
H1O H 0.698(14) 0.618(12) -0.074(9) 0.047 Uiso 0.50 1 d PD . .
N1 N 0.7423(5) 0.3570(5) 0.1368(4) 0.0401(9) Uani 1 1 d . . .
N2 N 0.5991(5) 0.4776(4) 0.2601(4) 0.0331(8) Uani 1 1 d . . .
N3 N 0.5296(5) 0.7094(4) 0.2857(4) 0.0341(8) Uani 1 1 d . . .
N4 N 0.5960(5) 0.8566(4) 0.1928(4) 0.0368(9) Uani 1 1 d . . .
C1 C 0.6230(6) 0.4328(5) 0.1384(4) 0.0326(9) Uani 1 1 d . . .
C2 C 0.7932(7) 0.3568(6) 0.2555(5) 0.0455(12) Uani 1 1 d . . .
H2B H 0.8758 0.3123 0.2779 0.055 Uiso 1 1 calc R . .
C3 C 0.7031(7) 0.4318(6) 0.3333(5) 0.0418(11) Uani 1 1 d . . .
H3B H 0.7095 0.4496 0.4201 0.050 Uiso 1 1 calc R . .
C4 C 0.4860(6) 0.5715(6) 0.3077(4) 0.0365(10) Uani 1 1 d . . .
H4B H 0.3699 0.5145 0.2628 0.044 Uiso 1 1 calc R . .
H4C H 0.4956 0.5985 0.3998 0.044 Uiso 1 1 calc R . .
C5 C 0.5414(6) 0.7081(5) 0.1695(4) 0.0309(9) Uani 1 1 d . . .
C6 C 0.5765(7) 0.8568(6) 0.3803(5) 0.0437(12) Uani 1 1 d . . .
H6A H 0.5786 0.8867 0.4683 0.052 Uiso 1 1 calc R . .
C7 C 0.6184(7) 0.9487(6) 0.3209(5) 0.0461(12) Uani 1 1 d . . .
H7A H 0.6559 1.0559 0.3598 0.055 Uiso 1 1 calc R . .
C8 C 0.8191(8) 0.2915(8) 0.0276(6) 0.0581(16) Uani 1 1 d . . .
H8A H 0.7642 0.3037 -0.0461 0.087 Uiso 1 1 calc R . .
H8B H 0.8063 0.1838 0.0065 0.087 Uiso 1 1 calc R . .
H8C H 0.9373 0.3438 0.0505 0.087 Uiso 1 1 calc R . .
C9 C 0.6344(8) 0.9162(6) 0.0980(5) 0.0491(13) Uani 1 1 d . . .
H9A H 0.6096 0.8323 0.0138 0.074 Uiso 1 1 calc R . .
H9B H 0.7523 0.9699 0.1214 0.074 Uiso 1 1 calc R . .
H9C H 0.5668 0.9859 0.0960 0.074 Uiso 1 1 calc R . .
P1 P 0.7852(9) 0.8499(7) 0.7320(7) 0.0423(3) Uani 0.6975(14) 1 d PD A 1
F1 F 0.6516(10) 0.7213(8) 0.6170(6) 0.129(5) Uani 0.6975(14) 1 d PD A 1
F2 F 0.9196(9) 0.8321(10) 0.6482(8) 0.170(6) Uani 0.6975(14) 1 d PD A 1
F3 F 0.9227(7) 0.9768(8) 0.8489(6) 0.125(3) Uani 0.6975(14) 1 d PD A 1
F4 F 0.6550(8) 0.8651(9) 0.8181(6) 0.096(2) Uani 0.6975(14) 1 d PD A 1
F5 F 0.7392(8) 0.9719(7) 0.6903(7) 0.092(2) Uani 0.6975(14) 1 d PD A 1
F6 F 0.8356(10) 0.7251(9) 0.7748(9) 0.121(4) Uani 0.6975(14) 1 d PD A 1
Re2 Re 0.7907(3) 0.8273(2) 0.7362(2) 0.0423(3) Uani 0.3025(14) 1 d PD A 2
O2 O 0.817(2) 0.746(2) 0.8426(15) 0.115(12) Uani 0.3025(14) 1 d PD A 2
O3 O 0.9716(18) 0.8747(19) 0.6990(19) 0.097(10) Uani 0.3025(14) 1 d PD A 2
O4 O 0.714(2) 0.9747(18) 0.7983(19) 0.138(13) Uani 0.3025(14) 1 d PD A 2
O5 O 0.6508(19) 0.6916(18) 0.6022(14) 0.051(5) Uani 0.3025(14) 1 d PD A 2
C1S C -0.0259(11) 0.7742(13) 0.3238(14) 0.130(5) Uani 1 1 d . . .
H1S1 H -0.1345 0.7149 0.3218 0.196 Uiso 1 1 calc R . .
H1S2 H -0.0159 0.7569 0.2367 0.196 Uiso 1 1 calc R . .
H1S3 H -0.0151 0.8818 0.3731 0.196 Uiso 1 1 calc R . .
C2S C 0.1045(8) 0.7280(8) 0.3829(7) 0.0605(16) Uani 1 1 d . . .
N1S N 0.2056(8) 0.6956(8) 0.4315(7) 0.0806(18) Uani 1 1 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 0.0756(2) 0.03018(15) 0.02051(14) 0.00598(10) -0.00114(12) 0.02172(13)
O1 0.0730(15) 0.0326(16) 0.0158(13) 0.0093(12) 0.0055(14) 0.0249(14)
N1 0.042(2) 0.037(2) 0.040(2) 0.0135(18) 0.0057(18) 0.0163(18)
N2 0.034(2) 0.0345(19) 0.0307(19) 0.0149(16) 0.0031(15) 0.0079(16)
N3 0.040(2) 0.0348(19) 0.0271(18) 0.0107(15) 0.0069(16) 0.0131(16)
N4 0.044(2) 0.0304(19) 0.032(2) 0.0110(16) 0.0018(17) 0.0101(17)
C1 0.033(2) 0.030(2) 0.033(2) 0.0119(18) 0.0061(18) 0.0062(18)
C2 0.041(3) 0.047(3) 0.052(3) 0.025(2) 0.001(2) 0.014(2)
C3 0.045(3) 0.041(3) 0.040(3) 0.021(2) -0.001(2) 0.009(2)
C4 0.043(3) 0.042(3) 0.028(2) 0.0159(19) 0.0114(19) 0.015(2)
C5 0.033(2) 0.031(2) 0.026(2) 0.0102(17) 0.0025(17) 0.0089(18)
C6 0.058(3) 0.040(3) 0.027(2) 0.0045(19) 0.005(2) 0.020(2)
C7 0.057(3) 0.031(2) 0.039(3) 0.004(2) 0.002(2) 0.014(2)
C8 0.059(4) 0.066(4) 0.055(3) 0.018(3) 0.019(3) 0.037(3)
C9 0.065(4) 0.035(3) 0.043(3) 0.019(2) 0.001(3) 0.005(2)
P1 0.0390(4) 0.0416(7) 0.0408(4) 0.0135(4) 0.0047(3) 0.0085(4)
F1 0.143(11) 0.121(9) 0.056(6) 0.010(5) -0.022(6) -0.034(7)
F2 0.178(11) 0.139(9) 0.259(15) 0.093(10) 0.185(12) 0.077(9)
F3 0.086(5) 0.104(6) 0.120(7) 0.021(5) -0.046(5) -0.022(4)
F4 0.092(5) 0.120(6) 0.084(5) 0.041(5) 0.046(4) 0.025(5)
F5 0.084(5) 0.091(5) 0.129(6) 0.076(5) 0.013(5) 0.031(4)
F6 0.084(5) 0.099(6) 0.221(13) 0.110(8) 0.018(7) 0.032(5)
Re2 0.0390(4) 0.0416(7) 0.0408(4) 0.0135(4) 0.0047(3) 0.0085(4)
O2 0.078(15) 0.13(2) 0.108(18) 0.078(16) -0.024(13) -0.058(14)
O3 0.054(10) 0.087(14) 0.20(3) 0.109(18) 0.020(13) 0.030(10)
O4 0.13(2) 0.095(17) 0.13(2) -0.022(17) -0.016(18) 0.086(17)
O5 0.048(11) 0.048(8) 0.041(10) 0.018(7) -0.012(8) -0.007(7)
C1S 0.056(5) 0.111(8) 0.234(14) 0.112(9) -0.023(7) -0.004(5)
C2S 0.044(3) 0.054(4) 0.073(4) 0.021(3) 0.003(3) 0.008(3)
N1S 0.067(4) 0.094(5) 0.081(4) 0.029(4) 0.015(3) 0.037(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
Re1 O1 1.946(4) 2_665 ?
Re1 O1 1.946(4) . ?
Re1 C5 2.154(4) . ?
Re1 C5 2.154(4) 2_665 ?
Re1 C1 2.155(5) . ?
Re1 C1 2.155(5) 2_665 ?
N1 C1 1.348(6) . ?
N1 C2 1.378(7) . ?
N1 C8 1.470(7) . ?
N2 C1 1.356(6) . ?
N2 C3 1.380(6) . ?
N2 C4 1.456(6) . ?
N3 C5 1.350(6) . ?
N3 C6 1.382(6) . ?
N3 C4 1.454(6) . ?
N4 C5 1.348(6) . ?
N4 C7 1.373(6) . ?
N4 C9 1.461(7) . ?
C2 C3 1.340(8) . ?
C6 C7 1.344(8) . ?
P1 F5 1.538(6) . ?
P1 F1 1.549(7) . ?
P1 F4 1.553(7) . ?
P1 F2 1.564(7) . ?
P1 F3 1.569(7) . ?
P1 F6 1.584(6) . ?
Re2 O4 1.643(12) . ?
Re2 O3 1.650(14) . ?
Re2 O5 1.703(13) . ?
Re2 O2 1.706(14) . ?
C1S C2S 1.440(11) . ?
C2S N1S 1.112(9) . ?

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
O1 Re1 O1 180.0(2) 2_665 . ?
O1 Re1 C5 90.60(15) 2_665 . ?
O1 Re1 C5 89.40(15) . . ?
O1 Re1 C5 89.40(15) 2_665 2_665 ?
O1 Re1 C5 90.60(15) . 2_665 ?
C5 Re1 C5 180.000(1) . 2_665 ?
O1 Re1 C1 92.30(15) 2_665 . ?
O1 Re1 C1 87.70(15) . . ?
C5 Re1 C1 81.42(16) . . ?
C5 Re1 C1 98.58(16) 2_665 . ?
O1 Re1 C1 87.70(15) 2_665 2_665 ?
O1 Re1 C1 92.30(15) . 2_665 ?
C5 Re1 C1 98.58(16) . 2_665 ?
C5 Re1 C1 81.42(16) 2_665 2_665 ?
C1 Re1 C1 180.0 . 2_665 ?
C1 N1 C2 110.9(4) . . ?
C1 N1 C8 125.7(4) . . ?
C2 N1 C8 123.2(5) . . ?
C1 N2 C3 111.4(4) . . ?
C1 N2 C4 123.3(4) . . ?
C3 N2 C4 125.2(4) . . ?
C5 N3 C6 111.2(4) . . ?
C5 N3 C4 123.3(4) . . ?
C6 N3 C4 125.3(4) . . ?
C5 N4 C7 111.2(4) . . ?
C5 N4 C9 125.9(4) . . ?
C7 N4 C9 122.8(4) . . ?
N1 C1 N2 104.2(4) . . ?
N1 C1 Re1 133.1(3) . . ?
N2 C1 Re1 122.4(3) . . ?
C3 C2 N1 107.4(4) . . ?
C2 C3 N2 106.1(5) . . ?
N3 C4 N2 109.1(4) . . ?
N4 C5 N3 104.3(4) . . ?
N4 C5 Re1 132.7(3) . . ?
N3 C5 Re1 122.7(3) . . ?
C7 C6 N3 106.2(4) . . ?
C6 C7 N4 107.0(4) . . ?
F5 P1 F1 91.2(4) . . ?
F5 P1 F4 91.5(5) . . ?
F1 P1 F4 90.5(4) . . ?
F5 P1 F2 90.4(4) . . ?
F1 P1 F2 90.2(4) . . ?
F4 P1 F2 178.0(6) . . ?
F5 P1 F3 90.3(4) . . ?
F1 P1 F3 178.5(5) . . ?
F4 P1 F3 89.9(4) . . ?
F2 P1 F3 89.3(4) . . ?
F5 P1 F6 179.1(5) . . ?
F1 P1 F6 89.3(4) . . ?
F4 P1 F6 89.3(6) . . ?
F2 P1 F6 88.8(4) . . ?
F3 P1 F6 89.2(5) . . ?
O4 Re2 O3 112.3(6) . . ?
O4 Re2 O5 109.7(6) . . ?
O3 Re2 O5 109.4(6) . . ?
O4 Re2 O2 109.6(6) . . ?
O3 Re2 O2 109.2(6) . . ?
O5 Re2 O2 106.6(6) . . ?
N1S C2S C1S 178.1(10) . . ?

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
O1 H1O O2 0.840(10) 2.04(8) 2.741(14) 140(10) 1_554
O1 H1O F6 0.840(10) 2.62(7) 3.314(8) 140(10) 1_554

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.248
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.108


data_b175
_database_code_depnum_ccdc_archive 'CCDC 842923'
#TrackingRef '2.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H41 F8.44 N8 O4.37 P1.41 Re1.59'
_chemical_formula_weight         1024.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   9.0425(10)
_cell_length_b                   17.8358(19)
_cell_length_c                   11.7838(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.328(3)
_cell_angle_gamma                90.00
_cell_volume                     1782.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    944
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      27.31

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            ORANGE
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1001
_exptl_absorpt_coefficient_mu    5.555
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.1786
_exptl_absorpt_correction_T_max  0.4196
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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 detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10532
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         24.99
_reflns_number_total             6224
_reflns_number_gt                6153
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '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.

The anions which appears to be a mixture of PF6- and ReO4-.
The disordered anion pairs were refined to a ratios of 66:34 and
74:26(PF6:ReO4). Restraints on geometries of the anions were applied because
proximity of the atoms led to poor L.S. convergence unless restraints were
applied. H2A was located from different map and refined with restraint in
bond length and thermal parameter.

Details of the restraints used:-
eadp re2 p1
eadp re3 p2
EADP O7 O8 O9 O10
EADP O3 O4 O5 O6
DELU 0.005 C1 N2 N8 C24
SADI 0.005 O7 O8 O7 O9 O7 O10 O8 O9 O8 O10 O9 O10
SADI 0.005 O3 O4 O3 O5 O3 O6 O4 O5 O4 O6 O5 O6
DFIX 1.65 0.002 Re2 O3 Re2 O4 Re2 O5 Re2 O6 Re3 O7 Re3 O8 Re3 O9 Re3 O10
DFIX 1.55 P1 F1 P1 F2 P1 F3 P1 F4 P1 F5 P1 F6
DFIX 1.55 P2 F7 P2 F8 P2 F9 P2 F10 P2 F11 P2 F12
SADI 0.005 F1 F2 F1 F4 F1 F5 F1 F6 F2 F3 F2 F5 F2 F6 F3 F4 F3 F5 F3 F6
SADI 0.005 F1 F3 F2 F4 F5 F6
SADI 0.005 F7 F8 F7 F10 F7 F11 F7 F12 F8 F9 F8 F11 F8 F12
SADI 0.005 F7 F9 F8 F10 F11 F12
DFIX 0.82 0.005 O2 H2A

PLAT420_ALERT_2_B D-H Without Acceptor O2 - H2A ... ? Response is:
The data were not good enough to locate the H atom
;

_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^)+(0.0100P)^2^+7.7741P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.107(13)
_refine_ls_number_reflns         6224
_refine_ls_number_parameters     515
_refine_ls_number_restraints     126
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1042
_refine_ls_wR_factor_gt          0.1039
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_restrained_S_all      1.265
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.1498(10) 0.5673(5) 0.8129(7) 0.0290(6) Uani 0.662(3) 1 d PD A 1
F1 F 0.1261(12) 0.4801(4) 0.7824(10) 0.097(5) Uani 0.662(3) 1 d PD A 1
F2 F 0.1327(11) 0.5827(6) 0.6766(7) 0.098(5) Uani 0.662(3) 1 d PD A 1
F3 F 0.1690(12) 0.6527(5) 0.8408(10) 0.098(5) Uani 0.662(3) 1 d PD A 1
F4 F 0.1778(19) 0.5493(7) 0.9491(8) 0.097(5) Uani 0.662(3) 1 d PD A 1
F5 F 0.3317(9) 0.5577(6) 0.8470(9) 0.093(5) Uani 0.662(3) 1 d PD A 1
F6 F -0.0369(9) 0.5752(5) 0.7751(9) 0.057(3) Uani 0.662(3) 1 d PD A 1
Re2 Re 0.1415(3) 0.57979(11) 0.83632(19) 0.0290(6) Uani 0.338(3) 1 d PD A 2
O3 O 0.2123(19) 0.5374(8) 0.9688(7) 0.029(3) Uani 0.338(3) 1 d PD A 2
O4 O -0.0526(4) 0.5838(9) 0.7934(15) 0.029(3) Uani 0.338(3) 1 d PD A 2
O5 O 0.2139(18) 0.6655(3) 0.8479(14) 0.029(3) Uani 0.338(3) 1 d PD A 2
O6 O 0.1919(18) 0.5322(6) 0.7353(11) 0.029(3) Uani 0.338(3) 1 d PD A 2
P2 P 0.8745(11) 0.2965(5) 0.7225(8) 0.0359(9) Uani 0.745(3) 1 d PD B 1
F7 F 0.8516(10) 0.2070(3) 0.6948(7) 0.051(3) Uani 0.745(3) 1 d PD B 1
F8 F 0.8634(8) 0.3116(4) 0.5871(6) 0.046(2) Uani 0.745(3) 1 d PD B 1
F9 F 0.9072(11) 0.3821(3) 0.7569(7) 0.052(2) Uani 0.745(3) 1 d PD B 1
F10 F 0.8925(11) 0.2796(5) 0.8618(5) 0.052(2) Uani 0.745(3) 1 d PD B 1
F11 F 1.0639(7) 0.2853(5) 0.7630(8) 0.059(3) Uani 0.745(3) 1 d PD B 1
F12 F 0.6899(7) 0.3061(4) 0.6885(7) 0.048(2) Uani 0.745(3) 1 d PD B 1
Re3 Re 0.8878(4) 0.28187(17) 0.7031(3) 0.0359(9) Uani 0.255(3) 1 d PD B 2
O7 O 0.807(4) 0.3204(16) 0.5684(13) 0.078(9) Uani 0.255(3) 1 d PD B 2
O8 O 0.840(4) 0.1923(5) 0.696(3) 0.078(9) Uani 0.255(3) 1 d PD B 2
O9 O 0.823(3) 0.3246(15) 0.801(2) 0.078(9) Uani 0.255(3) 1 d PD B 2
O10 O 1.0813(6) 0.2902(19) 0.747(3) 0.078(9) Uani 0.255(3) 1 d PD B 2
Re1 Re 0.52250(5) 0.42902(7) 0.27079(3) 0.03448(13) Uani 1 1 d . . .
O1 O 0.6988(7) 0.3752(4) 0.3257(6) 0.0276(14) Uani 1 1 d . . .
O2 O 0.3412(8) 0.4845(4) 0.2132(7) 0.0317(15) Uani 1 1 d D . .
H2A H 0.339(13) 0.527(3) 0.239(10) 0.038 Uiso 1 1 d D . .
N1 N 0.3805(10) 0.2630(5) 0.2858(8) 0.035(2) Uani 1 1 d . . .
N2 N 0.2632(10) 0.3197(5) 0.1185(9) 0.035(2) Uani 1 1 d U . .
N3 N 0.3810(9) 0.3874(5) -0.0024(8) 0.032(2) Uani 1 1 d . . .
N4 N 0.6234(8) 0.4113(4) 0.0331(7) 0.0261(19) Uani 1 1 d . . .
N5 N 0.4096(8) 0.4468(4) 0.5016(7) 0.0269(19) Uani 1 1 d . . .
N6 N 0.6541(9) 0.4725(5) 0.5402(7) 0.0266(18) Uani 1 1 d . . .
N7 N 0.7777(9) 0.5406(5) 0.4249(8) 0.0295(19) Uani 1 1 d . . .
N8 N 0.6667(10) 0.5947(5) 0.2535(8) 0.0333(18) Uani 1 1 d U . .
C1 C 0.3827(12) 0.3273(6) 0.2280(10) 0.034(2) Uani 1 1 d U . .
C2 C 0.2635(13) 0.2159(7) 0.2140(12) 0.046(3) Uani 1 1 d . . .
H2 H 0.2409 0.1682 0.2355 0.056 Uiso 1 1 calc R . .
C3 C 0.1895(12) 0.2497(6) 0.1103(11) 0.039(3) Uani 1 1 d . . .
H3 H 0.1059 0.2312 0.0454 0.047 Uiso 1 1 calc R . .
C4 C 0.2313(11) 0.3729(7) 0.0168(10) 0.039(3) Uani 1 1 d . . .
H4A H 0.1550 0.3517 -0.0558 0.047 Uiso 1 1 calc R . .
H4B H 0.1887 0.4193 0.0355 0.047 Uiso 1 1 calc R . .
C5 C 0.5124(10) 0.4115(4) 0.0863(9) 0.023(2) Uani 1 1 d . . .
C6 C 0.4069(12) 0.3706(6) -0.1074(9) 0.033(2) Uani 1 1 d . . .
H6 H 0.3340 0.3526 -0.1791 0.040 Uiso 1 1 calc R . .
C7 C 0.5617(12) 0.3861(5) -0.0844(10) 0.031(2) Uani 1 1 d . . .
H7 H 0.6159 0.3806 -0.1380 0.038 Uiso 1 1 calc R . .
C8 C 0.5034(14) 0.2406(6) 0.4005(10) 0.042(3) Uani 1 1 d . . .
H8 H 0.5504 0.2864 0.4441 0.050 Uiso 1 1 calc R . .
C9 C 0.6340(16) 0.1962(7) 0.3770(11) 0.051(3) Uani 1 1 d . . .
H9A H 0.5931 0.1488 0.3411 0.077 Uiso 1 1 calc R . .
H9B H 0.7188 0.1880 0.4521 0.077 Uiso 1 1 calc R . .
H9C H 0.6723 0.2239 0.3231 0.077 Uiso 1 1 calc R . .
C10 C 0.4301(18) 0.1966(7) 0.4799(12) 0.064(4) Uani 1 1 d . . .
H10A H 0.3342 0.2206 0.4779 0.096 Uiso 1 1 calc R . .
H10B H 0.5029 0.1953 0.5617 0.096 Uiso 1 1 calc R . .
H10C H 0.4075 0.1463 0.4497 0.096 Uiso 1 1 calc R . .
C11 C 0.7924(9) 0.4297(9) 0.0955(8) 0.0340(19) Uani 1 1 d . . .
H11 H 0.8014 0.4593 0.1677 0.041 Uiso 1 1 calc R . .
C12 C 0.8854(12) 0.3582(6) 0.1361(10) 0.040(3) Uani 1 1 d . . .
H12A H 0.8431 0.3306 0.1878 0.059 Uiso 1 1 calc R . .
H12B H 0.9938 0.3703 0.1798 0.059 Uiso 1 1 calc R . .
H12C H 0.8785 0.3284 0.0667 0.059 Uiso 1 1 calc R . .
C13 C 0.8533(14) 0.4776(7) 0.0126(12) 0.052(3) Uani 1 1 d . . .
H13A H 0.8676 0.4465 -0.0492 0.079 Uiso 1 1 calc R . .
H13B H 0.9522 0.5000 0.0596 0.079 Uiso 1 1 calc R . .
H13C H 0.7781 0.5163 -0.0242 0.079 Uiso 1 1 calc R . .
C14 C 0.5239(11) 0.4473(5) 0.4527(8) 0.029(2) Uani 1 1 d . . .
C15 C 0.4701(11) 0.4732(5) 0.6223(8) 0.028(2) Uani 1 1 d . . .
H15 H 0.4143 0.4791 0.6748 0.033 Uiso 1 1 calc R . .
C16 C 0.6233(12) 0.4882(5) 0.6465(9) 0.029(2) Uani 1 1 d . . .
H16 H 0.6950 0.5057 0.7192 0.035 Uiso 1 1 calc R . .
C17 C 0.8033(11) 0.4858(6) 0.5238(10) 0.035(2) Uani 1 1 d . . .
H17A H 0.8439 0.4393 0.5036 0.042 Uiso 1 1 calc R . .
H17B H 0.8796 0.5052 0.5980 0.042 Uiso 1 1 calc R . .
C18 C 0.6633(12) 0.5319(6) 0.3144(10) 0.029(2) Uani 1 1 d . . .
C19 C 0.8511(12) 0.6081(6) 0.4338(11) 0.037(2) Uani 1 1 d . . .
H19 H 0.9321 0.6269 0.5004 0.044 Uiso 1 1 calc R . .
C20 C 0.7818(13) 0.6422(6) 0.3257(11) 0.039(3) Uani 1 1 d . . .
H20 H 0.8072 0.6893 0.3039 0.047 Uiso 1 1 calc R . .
C21 C 0.2445(9) 0.4283(9) 0.4399(8) 0.0349(19) Uani 1 1 d . . .
H21 H 0.2363 0.4005 0.3663 0.042 Uiso 1 1 calc R . .
C22 C 0.1458(12) 0.4985(7) 0.4026(10) 0.041(3) Uani 1 1 d . . .
H22A H 0.1487 0.5259 0.4734 0.062 Uiso 1 1 calc R . .
H22B H 0.0388 0.4850 0.3569 0.062 Uiso 1 1 calc R . .
H22C H 0.1872 0.5292 0.3536 0.062 Uiso 1 1 calc R . .
C23 C 0.1849(14) 0.3777(7) 0.5190(12) 0.049(3) Uani 1 1 d . . .
H23A H 0.2521 0.3346 0.5432 0.074 Uiso 1 1 calc R . .
H23B H 0.0793 0.3618 0.4741 0.074 Uiso 1 1 calc R . .
H23C H 0.1857 0.4049 0.5896 0.074 Uiso 1 1 calc R . .
C24 C 0.5497(13) 0.6155(6) 0.1347(9) 0.036(2) Uani 1 1 d U . .
H24 H 0.4990 0.5698 0.0929 0.043 Uiso 1 1 calc R . .
C25 C 0.4253(15) 0.6653(6) 0.1542(11) 0.048(3) Uani 1 1 d . . .
H25A H 0.3756 0.6393 0.2026 0.072 Uiso 1 1 calc R . .
H25B H 0.3476 0.6779 0.0773 0.072 Uiso 1 1 calc R . .
H25C H 0.4737 0.7104 0.1949 0.072 Uiso 1 1 calc R . .
C26 C 0.6348(17) 0.6542(7) 0.0587(12) 0.053(3) Uani 1 1 d . . .
H26A H 0.6700 0.7029 0.0917 0.080 Uiso 1 1 calc R . .
H26B H 0.5637 0.6593 -0.0232 0.080 Uiso 1 1 calc R . .
H26C H 0.7240 0.6245 0.0599 0.080 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
P1 0.0303(7) 0.0257(10) 0.0374(12) -0.0047(7) 0.0198(7) 0.0015(6)
F1 0.103(12) 0.079(10) 0.100(11) -0.008(9) 0.022(9) 0.018(8)
F2 0.091(10) 0.135(14) 0.065(8) -0.007(9) 0.022(8) -0.045(10)
F3 0.086(11) 0.089(12) 0.110(13) 0.006(10) 0.024(10) -0.005(8)
F4 0.071(10) 0.108(13) 0.099(12) 0.029(10) 0.012(9) 0.005(9)
F5 0.063(8) 0.152(15) 0.065(8) 0.012(9) 0.023(7) -0.004(9)
F6 0.048(6) 0.060(8) 0.038(6) -0.033(6) -0.017(5) -0.008(6)
Re2 0.0303(7) 0.0257(10) 0.0374(12) -0.0047(7) 0.0198(7) 0.0015(6)
O3 0.040(7) 0.017(5) 0.043(7) -0.004(5) 0.031(6) -0.015(5)
O4 0.040(7) 0.017(5) 0.043(7) -0.004(5) 0.031(6) -0.015(5)
O5 0.040(7) 0.017(5) 0.043(7) -0.004(5) 0.031(6) -0.015(5)
O6 0.040(7) 0.017(5) 0.043(7) -0.004(5) 0.031(6) -0.015(5)
P2 0.0257(10) 0.0389(17) 0.0442(17) -0.0010(11) 0.0133(8) 0.0051(10)
F7 0.069(7) 0.033(5) 0.056(6) 0.007(4) 0.029(5) -0.005(4)
F8 0.045(6) 0.043(5) 0.060(6) 0.011(4) 0.030(5) -0.002(4)
F9 0.061(6) 0.032(5) 0.060(6) -0.007(4) 0.018(5) 0.011(4)
F10 0.057(5) 0.061(6) 0.045(5) 0.002(5) 0.025(5) 0.010(5)
F11 0.044(6) 0.044(6) 0.102(10) -0.003(6) 0.042(6) 0.022(5)
F12 0.033(4) 0.057(6) 0.060(6) 0.003(4) 0.022(4) 0.007(4)
Re3 0.0257(10) 0.0389(17) 0.0442(17) -0.0010(11) 0.0133(8) 0.0051(10)
O7 0.046(13) 0.066(15) 0.12(2) -0.056(15) 0.021(14) -0.008(11)
O8 0.046(13) 0.066(15) 0.12(2) -0.056(15) 0.021(14) -0.008(11)
O9 0.046(13) 0.066(15) 0.12(2) -0.056(15) 0.021(14) -0.008(11)
O10 0.046(13) 0.066(15) 0.12(2) -0.056(15) 0.021(14) -0.008(11)
Re1 0.0448(2) 0.03255(19) 0.0384(2) -0.0107(2) 0.03007(16) -0.0174(2)
O1 0.031(3) 0.027(4) 0.030(4) -0.002(3) 0.018(3) 0.001(3)
O2 0.037(4) 0.025(4) 0.043(4) -0.003(3) 0.025(3) 0.003(3)
N1 0.041(5) 0.032(5) 0.045(5) -0.004(4) 0.031(4) -0.005(4)
N2 0.037(5) 0.031(5) 0.049(5) -0.004(4) 0.029(4) -0.001(4)
N3 0.027(4) 0.031(5) 0.046(5) -0.001(4) 0.021(4) 0.000(3)
N4 0.027(4) 0.020(5) 0.039(4) 0.001(3) 0.021(4) 0.002(3)
N5 0.028(4) 0.026(5) 0.031(4) 0.002(3) 0.015(3) 0.003(3)
N6 0.022(4) 0.030(5) 0.030(5) 0.002(3) 0.011(4) 0.003(3)
N7 0.024(4) 0.033(5) 0.041(5) -0.002(4) 0.023(4) -0.004(3)
N8 0.038(4) 0.027(5) 0.047(5) -0.006(4) 0.029(4) -0.003(3)
C1 0.040(5) 0.032(6) 0.046(5) -0.008(5) 0.038(4) -0.003(4)
C2 0.045(6) 0.036(6) 0.073(9) -0.024(6) 0.039(7) -0.013(5)
C3 0.031(5) 0.038(6) 0.056(7) -0.015(6) 0.025(6) -0.009(5)
C4 0.019(5) 0.050(7) 0.053(7) -0.005(5) 0.019(5) 0.000(4)
C5 0.026(4) 0.012(5) 0.037(5) 0.000(3) 0.021(4) 0.001(3)
C6 0.035(5) 0.031(5) 0.028(5) -0.004(4) 0.004(5) -0.002(4)
C7 0.041(6) 0.020(5) 0.044(6) -0.001(4) 0.028(5) 0.002(4)
C8 0.061(7) 0.030(6) 0.044(6) -0.003(5) 0.030(6) -0.011(5)
C9 0.075(9) 0.038(7) 0.053(7) -0.002(5) 0.038(7) 0.002(6)
C10 0.116(12) 0.043(8) 0.051(8) -0.003(6) 0.053(9) -0.032(7)
C11 0.030(4) 0.041(5) 0.040(5) -0.001(7) 0.023(4) -0.006(6)
C12 0.029(5) 0.050(7) 0.044(6) -0.004(5) 0.017(5) 0.002(5)
C13 0.042(6) 0.059(8) 0.077(9) 0.000(7) 0.047(7) -0.004(5)
C14 0.030(5) 0.031(7) 0.024(5) 0.002(4) 0.007(4) 0.008(4)
C15 0.028(5) 0.033(6) 0.023(5) 0.002(4) 0.011(4) 0.004(4)
C16 0.033(5) 0.026(5) 0.029(5) -0.002(4) 0.012(5) 0.003(4)
C17 0.028(5) 0.037(6) 0.047(7) -0.004(5) 0.020(5) 0.001(4)
C18 0.035(5) 0.019(5) 0.047(6) -0.001(4) 0.031(5) -0.010(4)
C19 0.036(5) 0.026(5) 0.060(7) -0.006(5) 0.031(6) 0.003(4)
C20 0.049(6) 0.018(5) 0.072(8) -0.009(5) 0.047(7) -0.004(4)
C21 0.031(4) 0.035(5) 0.043(5) -0.013(7) 0.019(4) -0.004(6)
C22 0.028(5) 0.058(7) 0.041(6) -0.013(5) 0.015(5) 0.009(5)
C23 0.041(6) 0.053(7) 0.063(8) -0.003(6) 0.030(6) -0.011(5)
C24 0.052(6) 0.028(5) 0.037(5) 0.004(4) 0.027(4) -0.007(5)
C25 0.078(8) 0.027(6) 0.049(7) 0.010(5) 0.035(7) 0.014(5)
C26 0.087(9) 0.031(6) 0.061(8) -0.007(5) 0.050(8) -0.016(6)

_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
P1 F3 1.555(10) . ?
P1 F5 1.561(10) . ?
P1 F4 1.569(11) . ?
P1 F2 1.584(10) . ?
P1 F1 1.594(10) . ?
P1 F6 1.595(10) . ?
Re2 O5 1.649(2) . ?
Re2 O6 1.650(2) . ?
Re2 O3 1.650(2) . ?
Re2 O4 1.651(2) . ?
P2 F9 1.582(9) . ?
P2 F12 1.585(10) . ?
P2 F8 1.586(10) . ?
P2 F10 1.620(10) . ?
P2 F11 1.623(10) . ?
P2 F7 1.627(10) . ?
Re3 O7 1.650(2) . ?
Re3 O9 1.650(2) . ?
Re3 O8 1.650(2) . ?
Re3 O10 1.650(2) . ?
Re1 O1 1.779(6) . ?
Re1 O2 1.831(7) . ?
Re1 C14 2.164(9) . ?
Re1 C5 2.167(9) . ?
Re1 C1 2.168(11) . ?
Re1 C18 2.190(10) . ?
N1 C1 1.338(14) . ?
N1 C2 1.386(14) . ?
N1 C8 1.476(14) . ?
N2 C1 1.372(15) . ?
N2 C3 1.402(14) . ?
N2 C4 1.477(15) . ?
N3 C5 1.351(12) . ?
N3 C6 1.370(13) . ?
N3 C4 1.471(12) . ?
N4 C5 1.357(10) . ?
N4 C7 1.375(13) . ?
N4 C11 1.484(11) . ?
N5 C14 1.347(12) . ?
N5 C15 1.416(12) . ?
N5 C21 1.453(11) . ?
N6 C14 1.344(12) . ?
N6 C16 1.402(13) . ?
N6 C17 1.448(12) . ?
N7 C19 1.361(13) . ?
N7 C18 1.362(13) . ?
N7 C17 1.476(13) . ?
N8 C18 1.336(13) . ?
N8 C20 1.382(14) . ?
N8 C24 1.480(14) . ?
C2 C3 1.318(17) . ?
C6 C7 1.359(14) . ?
C8 C9 1.525(16) . ?
C8 C10 1.538(15) . ?
C11 C12 1.510(17) . ?
C11 C13 1.537(15) . ?
C15 C16 1.341(14) . ?
C19 C20 1.353(16) . ?
C21 C22 1.512(17) . ?
C21 C23 1.524(16) . ?
C24 C25 1.512(15) . ?
C24 C26 1.532(14) . ?

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
F3 P1 F5 91.3(5) . . ?
F3 P1 F4 91.0(5) . . ?
F5 P1 F4 86.2(8) . . ?
F3 P1 F2 90.5(5) . . ?
F5 P1 F2 90.2(5) . . ?
F4 P1 F2 176.1(8) . . ?
F3 P1 F1 178.7(7) . . ?
F5 P1 F1 89.9(5) . . ?
F4 P1 F1 89.6(5) . . ?
F2 P1 F1 89.0(5) . . ?
F3 P1 F6 90.2(5) . . ?
F5 P1 F6 178.3(7) . . ?
F4 P1 F6 94.8(8) . . ?
F2 P1 F6 88.9(5) . . ?
F1 P1 F6 88.6(5) . . ?
O5 Re2 O6 109.6(2) . . ?
O5 Re2 O3 109.5(2) . . ?
O6 Re2 O3 109.5(2) . . ?
O5 Re2 O4 109.5(2) . . ?
O6 Re2 O4 109.4(2) . . ?
O3 Re2 O4 109.4(2) . . ?
F9 P2 F12 92.7(6) . . ?
F9 P2 F8 92.0(6) . . ?
F12 P2 F8 92.0(5) . . ?
F9 P2 F10 88.6(6) . . ?
F12 P2 F10 90.1(6) . . ?
F8 P2 F10 177.8(7) . . ?
F9 P2 F11 87.6(6) . . ?
F12 P2 F11 177.5(8) . . ?
F8 P2 F11 90.5(5) . . ?
F10 P2 F11 87.4(7) . . ?
F9 P2 F7 176.1(8) . . ?
F12 P2 F7 90.4(5) . . ?
F8 P2 F7 90.3(4) . . ?
F10 P2 F7 89.0(5) . . ?
F11 P2 F7 89.2(4) . . ?
O7 Re3 O9 109.5(2) . . ?
O7 Re3 O8 109.5(2) . . ?
O9 Re3 O8 109.5(2) . . ?
O7 Re3 O10 109.5(2) . . ?
O9 Re3 O10 109.4(2) . . ?
O8 Re3 O10 109.5(2) . . ?
O1 Re1 O2 179.6(3) . . ?
O1 Re1 C14 91.4(3) . . ?
O2 Re1 C14 89.0(3) . . ?
O1 Re1 C5 90.4(3) . . ?
O2 Re1 C5 89.2(3) . . ?
C14 Re1 C5 178.0(4) . . ?
O1 Re1 C1 90.5(3) . . ?
O2 Re1 C1 89.5(4) . . ?
C14 Re1 C1 99.1(4) . . ?
C5 Re1 C1 80.1(3) . . ?
O1 Re1 C18 89.6(4) . . ?
O2 Re1 C18 90.4(3) . . ?
C14 Re1 C18 80.7(4) . . ?
C5 Re1 C18 100.1(3) . . ?
C1 Re1 C18 179.8(4) . . ?
C1 N1 C2 110.7(10) . . ?
C1 N1 C8 123.9(9) . . ?
C2 N1 C8 124.6(10) . . ?
C1 N2 C3 110.7(9) . . ?
C1 N2 C4 124.6(9) . . ?
C3 N2 C4 124.2(10) . . ?
C5 N3 C6 112.9(8) . . ?
C5 N3 C4 123.1(8) . . ?
C6 N3 C4 123.7(9) . . ?
C5 N4 C7 111.1(8) . . ?
C5 N4 C11 124.7(8) . . ?
C7 N4 C11 124.0(7) . . ?
C14 N5 C15 110.0(7) . . ?
C14 N5 C21 126.5(8) . . ?
C15 N5 C21 123.3(7) . . ?
C14 N6 C16 111.1(8) . . ?
C14 N6 C17 124.1(8) . . ?
C16 N6 C17 124.7(8) . . ?
C19 N7 C18 111.3(9) . . ?
C19 N7 C17 125.9(9) . . ?
C18 N7 C17 122.5(8) . . ?
C18 N8 C20 109.6(9) . . ?
C18 N8 C24 125.2(8) . . ?
C20 N8 C24 124.5(9) . . ?
N1 C1 N2 104.3(9) . . ?
N1 C1 Re1 135.2(8) . . ?
N2 C1 Re1 120.5(7) . . ?
C3 C2 N1 108.8(11) . . ?
C2 C3 N2 105.6(10) . . ?
N3 C4 N2 107.9(8) . . ?
N3 C5 N4 103.5(8) . . ?
N3 C5 Re1 122.8(6) . . ?
N4 C5 Re1 133.2(7) . . ?
C7 C6 N3 105.2(9) . . ?
C6 C7 N4 107.3(9) . . ?
N1 C8 C9 111.0(9) . . ?
N1 C8 C10 110.4(10) . . ?
C9 C8 C10 111.7(10) . . ?
N4 C11 C12 109.5(11) . . ?
N4 C11 C13 110.0(8) . . ?
C12 C11 C13 112.8(8) . . ?
N6 C14 N5 105.8(8) . . ?
N6 C14 Re1 120.8(7) . . ?
N5 C14 Re1 133.0(7) . . ?
C16 C15 N5 106.9(8) . . ?
C15 C16 N6 106.3(9) . . ?
N6 C17 N7 108.4(8) . . ?
N8 C18 N7 105.5(8) . . ?
N8 C18 Re1 134.1(8) . . ?
N7 C18 Re1 120.4(7) . . ?
C20 C19 N7 105.7(10) . . ?
C19 C20 N8 107.9(10) . . ?
N5 C21 C22 111.0(11) . . ?
N5 C21 C23 110.4(8) . . ?
C22 C21 C23 111.7(8) . . ?
N8 C24 C25 109.2(9) . . ?
N8 C24 C26 109.1(9) . . ?
C25 C24 C26 112.1(9) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.662
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.129


data_a051
_database_code_depnum_ccdc_archive 'CCDC 882460'
#TrackingRef '3.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H53 F7.8 N12 O4.8 P1.30 Re1.70'
_chemical_formula_weight         1378.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           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                   11.6582(6)
_cell_length_b                   11.1157(6)
_cell_length_c                   22.0292(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.7910(10)
_cell_angle_gamma                90.00
_cell_volume                     2783.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    2870
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      21.31

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            ORANGE
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1385.20
_exptl_absorpt_coefficient_mu    3.815
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5805
_exptl_absorpt_correction_T_max  0.7280
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(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 detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19182
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6379
_reflns_number_gt                4936
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '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.

The anion which appears to be a mixture of PF6- and ReO4-. The disordered
anion pair were refined to a ratio of 0.65 PF6- to 0.35 ReO4-.
Restraints on geometries of the anions were applied because proximity of the
atoms led to poor L.S. convergence unless restraints were applied.
Details of restraints:-
SADI O1R O2R O2R O3R O3R O4R O1R O3R O1R O4R
DFIX 1.72 0.01 RE2 O1R RE2 O2R RE2 O3R RE2 O4R
DFIX 1.45 C3S C4S
DFIX 1.13 C4S N2S
DFIX 2.23 0.01 F1 F2 F2 F3 F3 F4 F4 F1 F5 F1 F5 F2 F5 F3 F5 F4
DFIX 2.23 0.01 F6 F1 F6 F2 F6 F3 F6 F4
DFIX 1.57 0.010 P1 F1 P1 F2 P1 F3 P1 F4 P1 F5 P1 F6
DFIX 0.85 0.001 O1 H91
EADP F5 F6
EADP F2 F4
EADP F1 F3
ISOR 0.005 0.01 P1 F5
SIMU 0.01 P1 F5
ISOR 0.02 0.03 O1R O2R O3R O4R
ISOR 0.02 0.03 N2S C3S
ISOR 0.02 0.03 $C
For PLAT420_ALERT_2_B D-H Without Acceptor O1 - *H91 ... ? Response is:
There is a H bond to N atom of the acetonitrile solvent.
For PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C9.
Response is: The C9 has high thermal motion.
;

_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^)+(0.0512P)^2^+5.4129P] 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         6379
_refine_ls_number_parameters     380
_refine_ls_number_restraints     239
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1373
_refine_ls_wR_factor_gt          0.1285
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C3S C 0.4740(18) 0.8877(17) 0.8956(9) 0.222(9) Uani 1 1 d DU . .
H3S1 H 0.4788 0.9293 0.8575 0.333 Uiso 1 1 calc R . .
H3S2 H 0.4389 0.8091 0.8855 0.333 Uiso 1 1 calc R . .
H3S3 H 0.5524 0.8784 0.9215 0.333 Uiso 1 1 calc R . .
C4S C 0.4027(16) 0.9566(15) 0.9287(9) 0.152(6) Uani 1 1 d DU . .
N2S N 0.3465(12) 1.0086(12) 0.9564(9) 0.175(7) Uani 1 1 d DU . .
P1 P 0.8035(7) 0.4556(7) 0.1861(4) 0.062(3) Uani 0.6498(18) 1 d PDU A 1
F1 F 0.7598(7) 0.4915(8) 0.1145(3) 0.101(2) Uani 0.6498(18) 1 d PD A 1
F2 F 0.6768(6) 0.4760(8) 0.1966(5) 0.089(2) Uani 0.6498(18) 1 d PD A 1
F3 F 0.8516(8) 0.4350(9) 0.2576(3) 0.101(2) Uani 0.6498(18) 1 d PD A 1
F4 F 0.9341(5) 0.4500(7) 0.1758(4) 0.089(2) Uani 0.6498(18) 1 d PD A 1
F5 F 0.8279(8) 0.6001(7) 0.1980(5) 0.100(2) Uani 0.6498(18) 1 d PDU A 1
F6 F 0.7848(7) 0.3239(6) 0.1711(4) 0.100(2) Uani 0.6498(18) 1 d PD A 1
Re2 Re 0.80255(19) 0.4767(2) 0.18913(11) 0.0484(5) Uani 0.3502(18) 1 d PD A 2
O1R O 0.8155(19) 0.6291(9) 0.1989(11) 0.121(10) Uani 0.3502(18) 1 d PDU A 2
O2R O 0.9010(17) 0.399(2) 0.2435(12) 0.146(12) Uani 0.3502(18) 1 d PDU A 2
O3R O 0.6621(10) 0.4261(16) 0.1831(10) 0.089(8) Uani 0.3502(18) 1 d PDU A 2
O4R O 0.856(2) 0.438(2) 0.1249(9) 0.111(7) Uani 0.3502(18) 1 d PDU A 2
Re1 Re 0.0000 1.0000 0.0000 0.03627(13) Uani 1 2 d S . .
O1 O 0.1526(4) 1.0330(4) 0.0350(2) 0.0425(11) Uani 1 1 d D . .
H91 H 0.222(5) 1.062(14) 0.040(8) 0.07(6) Uiso 0.50 1 d PD . .
N1 N -0.0213(5) 1.0776(5) 0.1386(2) 0.0412(13) Uani 1 1 d . . .
N2 N -0.0978(5) 0.9077(5) 0.1112(2) 0.0428(13) Uani 1 1 d . . .
N3 N -0.0401(5) 0.7479(5) 0.0538(2) 0.0427(13) Uani 1 1 d . . .
N4 N 0.1106(5) 0.7311(5) 0.0129(2) 0.0424(13) Uani 1 1 d . . .
C1 C -0.0408(5) 1.0013(6) 0.0913(3) 0.0400(14) Uani 1 1 d U . .
C2 C -0.0667(7) 1.0365(8) 0.1871(3) 0.056(2) Uani 1 1 d U . .
H2A H -0.0633 1.0761 0.2251 0.067 Uiso 1 1 calc R . .
C3 C -0.1159(6) 0.9319(8) 0.1706(3) 0.0521(18) Uani 1 1 d U . .
H3A H -0.1554 0.8829 0.1942 0.062 Uiso 1 1 calc R . .
C4 C 0.0457(6) 1.1904(7) 0.1414(3) 0.0522(18) Uani 1 1 d U . .
H4A H -0.0022 1.2565 0.1517 0.063 Uiso 1 1 calc R . .
H4B H 0.0611 1.2068 0.1002 0.063 Uiso 1 1 calc R . .
C5 C 0.1615(4) 1.1875(5) 0.1887(2) 0.0476(17) Uani 1 1 d GU . .
C6 C 0.2472(5) 1.1032(5) 0.1841(2) 0.079(3) Uani 1 1 d GU . .
H6A H 0.2331 1.0463 0.1517 0.095 Uiso 1 1 calc R . .
C7 C 0.3539(4) 1.1029(6) 0.2274(3) 0.081(3) Uani 1 1 d GU . .
H7A H 0.4119 1.0459 0.2243 0.097 Uiso 1 1 calc R . .
C8 C 0.3748(4) 1.1869(6) 0.2754(3) 0.082(3) Uani 1 1 d GU . .
H8A H 0.4469 1.1867 0.3047 0.098 Uiso 1 1 calc R . .
C9 C 0.2891(6) 1.2712(6) 0.2799(3) 0.136(5) Uani 1 1 d GU . .
H9A H 0.3032 1.3280 0.3123 0.163 Uiso 1 1 calc R . .
C10 C 0.1824(5) 1.2715(5) 0.2366(3) 0.111(4) Uani 1 1 d GU . .
H10A H 0.1244 1.3285 0.2397 0.134 Uiso 1 1 calc R . .
C11 C -0.1364(6) 0.7993(7) 0.0752(3) 0.0485(17) Uani 1 1 d U . .
H11A H -0.1665 0.7409 0.1012 0.058 Uiso 1 1 calc R . .
H11B H -0.2001 0.8192 0.0395 0.058 Uiso 1 1 calc R . .
C12 C 0.0285(5) 0.8111(6) 0.0224(3) 0.0387(15) Uani 1 1 d U . .
C13 C -0.0017(7) 0.6308(7) 0.0613(3) 0.056(2) Uani 1 1 d U . .
H13A H -0.0355 0.5689 0.0807 0.068 Uiso 1 1 calc R . .
C14 C 0.0904(7) 0.6209(7) 0.0367(4) 0.058(2) Uani 1 1 d U . .
H14A H 0.1349 0.5507 0.0355 0.069 Uiso 1 1 calc R . .
C15 C 0.2100(6) 0.7560(7) -0.0159(3) 0.055(2) Uani 1 1 d U . .
H15A H 0.2037 0.8385 -0.0320 0.066 Uiso 1 1 calc R . .
H15B H 0.2068 0.7013 -0.0511 0.066 Uiso 1 1 calc R . .
C16 C 0.3256(6) 0.7410(7) 0.0296(4) 0.0516(18) Uani 1 1 d U . .
C17 C 0.4132(7) 0.6708(7) 0.0151(4) 0.064(2) Uani 1 1 d U . .
H17A H 0.3981 0.6287 -0.0229 0.077 Uiso 1 1 calc R . .
C18 C 0.5217(7) 0.6607(9) 0.0544(5) 0.082(3) Uani 1 1 d U . .
H18A H 0.5812 0.6145 0.0431 0.098 Uiso 1 1 calc R . .
C19 C 0.5421(8) 0.7196(9) 0.1112(5) 0.081(3) Uani 1 1 d U . .
H19A H 0.6151 0.7109 0.1393 0.097 Uiso 1 1 calc R . .
C20 C 0.4586(9) 0.7889(9) 0.1263(4) 0.086(3) Uani 1 1 d U . .
H20A H 0.4737 0.8308 0.1643 0.103 Uiso 1 1 calc R . .
C21 C 0.3497(8) 0.7986(9) 0.0855(4) 0.083(3) Uani 1 1 d U . .
H21A H 0.2911 0.8461 0.0968 0.100 Uiso 1 1 calc R . .
N1S N 0.2563(8) 0.3467(8) 0.0553(4) 0.099(3) Uani 1 1 d . . .
C1S C 0.3119(8) 0.3870(8) 0.0962(5) 0.075(3) Uani 1 1 d U . .
C2S C 0.3778(12) 0.4464(13) 0.1521(5) 0.129(5) Uani 1 1 d U . .
H2S1 H 0.3583 0.5313 0.1505 0.194 Uiso 1 1 calc R . .
H2S2 H 0.4614 0.4369 0.1546 0.194 Uiso 1 1 calc R . .
H2S3 H 0.3576 0.4105 0.1885 0.194 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
C3S 0.250(17) 0.196(16) 0.267(17) 0.076(14) 0.158(15) 0.015(13)
C4S 0.125(11) 0.140(12) 0.207(15) 0.073(11) 0.071(11) 0.027(9)
N2S 0.091(9) 0.152(12) 0.285(18) 0.067(11) 0.047(10) 0.026(7)
P1 0.047(3) 0.095(5) 0.037(3) -0.006(3) -0.003(2) 0.037(3)
F1 0.096(5) 0.145(7) 0.051(4) 0.012(4) -0.004(3) 0.027(4)
F2 0.061(4) 0.094(5) 0.117(6) 0.010(4) 0.033(4) 0.021(3)
F3 0.096(5) 0.145(7) 0.051(4) 0.012(4) -0.004(3) 0.027(4)
F4 0.061(4) 0.094(5) 0.117(6) 0.010(4) 0.033(4) 0.021(3)
F5 0.085(4) 0.089(4) 0.126(5) -0.010(4) 0.024(4) -0.006(4)
F6 0.085(4) 0.089(4) 0.126(5) -0.010(4) 0.024(4) -0.006(4)
Re2 0.0409(9) 0.0540(8) 0.0495(10) 0.0060(6) 0.0079(6) 0.0063(6)
O1R 0.110(17) 0.114(17) 0.116(17) -0.035(14) -0.022(13) 0.062(14)
O2R 0.094(17) 0.18(2) 0.15(2) 0.046(18) -0.011(15) 0.037(16)
O3R 0.086(14) 0.077(14) 0.106(16) 0.010(12) 0.025(11) -0.028(11)
O4R 0.16(2) 0.111(15) 0.076(13) -0.010(12) 0.047(14) -0.007(15)
Re1 0.0375(2) 0.0400(2) 0.0321(2) 0.00154(16) 0.00931(14) 0.00709(17)
O1 0.032(2) 0.053(3) 0.041(3) 0.003(2) 0.004(2) 0.002(2)
N1 0.034(3) 0.053(3) 0.034(3) -0.007(3) 0.002(2) 0.007(2)
N2 0.033(3) 0.057(4) 0.038(3) 0.002(3) 0.008(2) 0.002(3)
N3 0.038(3) 0.043(3) 0.042(3) 0.001(2) -0.002(2) -0.001(2)
N4 0.037(3) 0.048(3) 0.036(3) -0.003(2) -0.006(2) 0.011(2)
C1 0.031(3) 0.045(3) 0.044(3) -0.007(3) 0.009(3) -0.003(3)
C2 0.059(5) 0.076(5) 0.032(4) -0.006(3) 0.009(3) 0.014(4)
C3 0.049(4) 0.076(5) 0.033(4) 0.007(4) 0.013(3) 0.007(4)
C4 0.053(4) 0.053(4) 0.044(4) -0.007(3) -0.003(3) 0.009(3)
C5 0.051(4) 0.052(4) 0.035(4) -0.004(3) 0.001(3) -0.001(3)
C6 0.065(5) 0.080(6) 0.075(6) -0.024(5) -0.023(5) 0.016(5)
C7 0.066(6) 0.081(6) 0.082(6) -0.005(5) -0.012(5) 0.016(5)
C8 0.056(5) 0.106(7) 0.069(6) -0.009(5) -0.017(4) -0.002(5)
C9 0.100(8) 0.179(12) 0.103(8) -0.078(8) -0.035(7) 0.025(8)
C10 0.095(8) 0.139(9) 0.082(7) -0.058(7) -0.020(6) 0.035(7)
C11 0.043(4) 0.058(4) 0.043(4) 0.008(3) 0.006(3) -0.011(3)
C12 0.031(3) 0.045(4) 0.035(3) -0.008(3) -0.003(3) 0.006(3)
C13 0.056(5) 0.046(4) 0.055(5) 0.006(3) -0.012(4) -0.005(4)
C14 0.051(4) 0.045(4) 0.065(5) -0.011(4) -0.014(4) 0.010(3)
C15 0.041(4) 0.072(5) 0.047(4) -0.008(4) -0.001(3) 0.021(4)
C16 0.040(4) 0.055(4) 0.054(4) 0.001(4) -0.002(3) 0.007(3)
C17 0.049(4) 0.062(5) 0.078(6) 0.000(4) 0.007(4) 0.016(4)
C18 0.043(5) 0.097(7) 0.104(7) 0.004(6) 0.014(5) 0.026(5)
C19 0.043(5) 0.084(6) 0.106(8) 0.026(6) -0.004(5) -0.003(4)
C20 0.076(6) 0.091(7) 0.071(6) -0.019(5) -0.025(5) 0.002(5)
C21 0.067(6) 0.094(7) 0.075(6) -0.025(5) -0.015(5) 0.034(5)
N1S 0.099(7) 0.080(6) 0.093(6) -0.010(5) -0.029(5) 0.007(5)
C1S 0.067(6) 0.066(6) 0.080(6) 0.007(5) -0.011(5) -0.005(4)
C2S 0.123(10) 0.131(10) 0.113(10) 0.000(8) -0.020(8) -0.047(9)

_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
C3S C4S 1.441(15) . ?
C4S N2S 1.147(15) . ?
P1 F6 1.506(8) . ?
P1 F2 1.561(8) . ?
P1 F3 1.566(8) . ?
P1 F4 1.590(8) . ?
P1 F1 1.597(8) . ?
P1 F5 1.641(8) . ?
Re2 O2R 1.700(9) . ?
Re2 O3R 1.708(9) . ?
Re2 O1R 1.711(10) . ?
Re2 O4R 1.725(9) . ?
Re1 O1 1.813(4) . ?
Re1 O1 1.813(4) 3_575 ?
Re1 C12 2.166(7) 3_575 ?
Re1 C12 2.166(7) . ?
Re1 C1 2.166(7) 3_575 ?
Re1 C1 2.166(7) . ?
N1 C1 1.325(8) . ?
N1 C2 1.371(9) . ?
N1 C4 1.471(9) . ?
N2 C1 1.359(8) . ?
N2 C3 1.397(8) . ?
N2 C11 1.458(9) . ?
N3 C12 1.362(8) . ?
N3 C13 1.375(9) . ?
N3 C11 1.430(9) . ?
N4 C12 1.356(8) . ?
N4 C14 1.373(9) . ?
N4 C15 1.466(9) . ?
C2 C3 1.311(11) . ?
C4 C5 1.512(7) . ?
C5 C6 1.3900 . ?
C5 C10 1.3900 . ?
C6 C7 1.3900 . ?
C7 C8 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C13 C14 1.311(11) . ?
C15 C16 1.500(9) . ?
C16 C21 1.360(11) . ?
C16 C17 1.378(10) . ?
C17 C18 1.370(11) . ?
C18 C19 1.385(13) . ?
C19 C20 1.341(13) . ?
C20 C21 1.387(11) . ?
N1S C1S 1.082(10) . ?
C1S C2S 1.458(13) . ?

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
N2S C4S C3S 178(2) . . ?
F6 P1 F2 94.5(5) . . ?
F6 P1 F3 94.6(5) . . ?
F2 P1 F3 90.7(5) . . ?
F6 P1 F4 91.5(5) . . ?
F2 P1 F4 173.9(6) . . ?
F3 P1 F4 89.8(5) . . ?
F6 P1 F1 91.5(5) . . ?
F2 P1 F1 90.3(5) . . ?
F3 P1 F1 173.7(6) . . ?
F4 P1 F1 88.5(5) . . ?
F6 P1 F5 175.9(6) . . ?
F2 P1 F5 88.3(5) . . ?
F3 P1 F5 88.4(5) . . ?
F4 P1 F5 85.6(5) . . ?
F1 P1 F5 85.4(5) . . ?
O2R Re2 O3R 111.9(8) . . ?
O2R Re2 O1R 112.8(9) . . ?
O3R Re2 O1R 113.1(7) . . ?
O2R Re2 O4R 98.0(15) . . ?
O3R Re2 O4R 111.8(8) . . ?
O1R Re2 O4R 108.2(8) . . ?
O1 Re1 O1 180.000(1) . 3_575 ?
O1 Re1 C12 89.3(2) . 3_575 ?
O1 Re1 C12 90.7(2) 3_575 3_575 ?
O1 Re1 C12 90.7(2) . . ?
O1 Re1 C12 89.3(2) 3_575 . ?
C12 Re1 C12 180.0(3) 3_575 . ?
O1 Re1 C1 90.0(2) . 3_575 ?
O1 Re1 C1 90.0(2) 3_575 3_575 ?
C12 Re1 C1 81.3(2) 3_575 3_575 ?
C12 Re1 C1 98.7(2) . 3_575 ?
O1 Re1 C1 90.0(2) . . ?
O1 Re1 C1 90.0(2) 3_575 . ?
C12 Re1 C1 98.7(2) 3_575 . ?
C12 Re1 C1 81.3(2) . . ?
C1 Re1 C1 180.000(1) 3_575 . ?
C1 N1 C2 111.8(6) . . ?
C1 N1 C4 125.1(6) . . ?
C2 N1 C4 123.0(6) . . ?
C1 N2 C3 110.0(6) . . ?
C1 N2 C11 124.8(6) . . ?
C3 N2 C11 125.2(6) . . ?
C12 N3 C13 109.7(6) . . ?
C12 N3 C11 123.6(6) . . ?
C13 N3 C11 126.6(6) . . ?
C12 N4 C14 109.9(6) . . ?
C12 N4 C15 126.5(6) . . ?
C14 N4 C15 123.5(6) . . ?
N1 C1 N2 104.3(6) . . ?
N1 C1 Re1 134.5(5) . . ?
N2 C1 Re1 121.3(5) . . ?
C3 C2 N1 107.5(6) . . ?
C2 C3 N2 106.4(7) . . ?
N1 C4 C5 113.3(6) . . ?
C6 C5 C10 120.0 . . ?
C6 C5 C4 120.7(4) . . ?
C10 C5 C4 119.3(4) . . ?
C7 C6 C5 120.0 . . ?
C6 C7 C8 120.0 . . ?
C9 C8 C7 120.0 . . ?
C8 C9 C10 120.0 . . ?
C9 C10 C5 120.0 . . ?
N3 C11 N2 109.8(5) . . ?
N4 C12 N3 104.7(6) . . ?
N4 C12 Re1 132.8(5) . . ?
N3 C12 Re1 122.5(4) . . ?
C14 C13 N3 107.7(7) . . ?
C13 C14 N4 107.9(7) . . ?
N4 C15 C16 111.6(6) . . ?
C21 C16 C17 117.5(7) . . ?
C21 C16 C15 121.8(7) . . ?
C17 C16 C15 120.7(7) . . ?
C18 C17 C16 121.8(8) . . ?
C17 C18 C19 118.8(8) . . ?
C20 C19 C18 120.4(8) . . ?
C19 C20 C21 119.6(9) . . ?
C16 C21 C20 121.7(8) . . ?
N1S C1S C2S 175.1(13) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.759
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.132