# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2014

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#                 Cambridge Crystallographic Data Centre
#                                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
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  from this site to visualise CIF-encoded structures and 
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data_c:[tc(benzene)2](pf6)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Tc(benzol)2]PF6'
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Tc, F6 P'
_chemical_formula_sum            'C12 H12 F6 P Tc'
_chemical_formula_weight         399.19

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'
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'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   13.8831(7)
_cell_length_b                   9.8745(5)
_cell_length_c                   9.7190(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.232(5)
_cell_angle_gamma                90.00
_cell_volume                     1328.74(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    2629
_cell_measurement_theta_min      2.5600
_cell_measurement_theta_max      32.4940

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7193
_exptl_absorpt_correction_T_max  0.8239
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 none 
;

_diffrn_ambient_temperature      183(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  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7418
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.53
_diffrn_reflns_theta_max         28.28
_reflns_number_total             3296
_reflns_number_gt                2139
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0345P)²+1.0818P] where P=(Fo²+2Fc²)/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         3296
_refine_ls_number_parameters     184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0904
_refine_ls_wR_factor_gt          0.0757
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.003
_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
Tc1 Tc 0.5000 -0.5000 0.5000 0.02494(11) Uani 1 2 d S . .
Tc2 Tc 0.0000 0.0000 0.0000 0.02492(11) Uani 1 2 d S . .
C1 C 0.3698(3) -0.4637(4) 0.6140(4) 0.0566(10) Uani 1 1 d . . .
H1A H 0.3419 -0.3810 0.6411 0.068 Uiso 1 1 calc R . .
C2 C 0.4380(3) -0.5266(4) 0.7029(4) 0.0508(9) Uani 1 1 d . . .
H2A H 0.4576 -0.4867 0.7895 0.061 Uiso 1 1 calc R . .
C3 C 0.4782(3) -0.6506(4) 0.6637(4) 0.0538(9) Uani 1 1 d . . .
H3A H 0.5253 -0.6948 0.7236 0.065 Uiso 1 1 calc R . .
C4 C 0.4481(3) -0.7086(3) 0.5353(4) 0.0546(10) Uani 1 1 d . . .
H4A H 0.4745 -0.7927 0.5089 0.065 Uiso 1 1 calc R . .
C5 C 0.3798(3) -0.6428(4) 0.4472(4) 0.0545(10) Uani 1 1 d . . .
H5A H 0.3594 -0.6825 0.3608 0.065 Uiso 1 1 calc R . .
C6 C 0.3409(2) -0.5190(4) 0.4845(4) 0.0547(10) Uani 1 1 d . . .
H6A H 0.2956 -0.4729 0.4233 0.066 Uiso 1 1 calc R . .
C11A C -0.0577(6) 0.0621(10) 0.1927(7) 0.125(3) Uani 1 1 d . A 1
H11A H -0.1083 0.0212 0.2386 0.150 Uiso 1 1 calc R A 1
C12A C 0.0344(8) 0.0215(8) 0.2210(5) 0.140(3) Uani 1 1 d . A 1
H12A H 0.0483 -0.0483 0.2868 0.168 Uiso 1 1 calc R A 1
C13A C 0.1076(4) 0.0794(9) 0.1561(8) 0.111(3) Uani 1 1 d . A 1
H13A H 0.1722 0.0516 0.1797 0.134 Uiso 1 1 calc R A 1
C14A C 0.0897(6) 0.1772(7) 0.0575(9) 0.120(3) Uani 1 1 d . A 1
H14A H 0.1408 0.2155 0.0106 0.144 Uiso 1 1 calc R A 1
C15A C -0.0047(7) 0.2189(5) 0.0278(8) 0.135(3) Uani 1 1 d . A 1
H15A H -0.0195 0.2862 -0.0404 0.162 Uiso 1 1 calc R A 1
C16A C -0.0779(4) 0.1608(7) 0.0991(10) 0.118(3) Uani 1 1 d . A 1
H16A H -0.1426 0.1910 0.0817 0.141 Uiso 1 1 calc R A 1
P1 P 0.27133(7) -0.03024(10) 0.53125(10) 0.0402(2) Uani 1 1 d . . .
F1 F 0.15612(16) -0.0253(2) 0.5152(3) 0.0676(7) Uani 1 1 d . . .
F2 F 0.2718(2) -0.1423(3) 0.4165(3) 0.0874(9) Uani 1 1 d . . .
F3 F 0.2667(2) -0.1413(3) 0.6467(3) 0.0842(8) Uani 1 1 d . . .
F4 F 0.38559(17) -0.0310(3) 0.5477(3) 0.0833(8) Uani 1 1 d . . .
F5 F 0.26926(19) 0.0852(3) 0.6449(2) 0.0798(8) Uani 1 1 d . . .
F6 F 0.27450(17) 0.0831(3) 0.4158(2) 0.0715(7) Uani 1 1 d . . .


_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
Tc1 C6 2.210(3) 3_646 ?
Tc1 C6 2.210(3) . ?
Tc1 C1 2.217(3) 3_646 ?
Tc1 C1 2.217(3) . ?
Tc1 C5 2.216(3) . ?
Tc1 C5 2.217(3) 3_646 ?
Tc1 C3 2.215(3) 3_646 ?
Tc1 C3 2.215(3) . ?
Tc1 C4 2.217(3) 3_646 ?
Tc1 C4 2.217(3) . ?
Tc1 C2 2.225(3) 3_646 ?
Tc1 C2 2.225(3) . ?
Tc2 C12A 2.176(5) 3 ?
Tc2 C12A 2.176(5) . ?
Tc2 C11A 2.178(5) 3 ?
Tc2 C11A 2.178(5) . ?
Tc2 C16A 2.184(4) . ?
Tc2 C16A 2.184(4) 3 ?
Tc2 C15A 2.180(5) . ?
Tc2 C15A 2.180(5) 3 ?
Tc2 C13A 2.194(4) . ?
Tc2 C13A 2.194(4) 3 ?
Tc2 C14A 2.196(5) 3 ?
Tc2 C14A 2.196(5) . ?
C1 C2 1.381(6) . ?
C1 C6 1.403(5) . ?
C1 H1A 0.9500 . ?
C2 C3 1.410(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.408(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.395(5) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C11A C12A 1.348(10) . ?
C11A C16A 1.348(10) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.361(10) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.370(9) . ?
C13A H13A 0.9500 . ?
C14A C15A 1.384(9) . ?
C14A H14A 0.9500 . ?
C15A C16A 1.395(9) . ?
C15A H15A 0.9500 . ?
C16A H16A 0.9500 . ?
P1 F2 1.572(2) . ?
P1 F3 1.574(2) . ?
P1 F4 1.583(2) . ?
P1 F6 1.588(2) . ?
P1 F5 1.589(2) . ?
P1 F1 1.596(2) . ?

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
C6 Tc1 C6 180.0 3_646 . ?
C6 Tc1 C1 36.95(14) 3_646 3_646 ?
C6 Tc1 C1 143.05(14) . 3_646 ?
C6 Tc1 C1 143.05(14) 3_646 . ?
C6 Tc1 C1 36.95(14) . . ?
C1 Tc1 C1 180.0 3_646 . ?
C6 Tc1 C5 143.27(13) 3_646 . ?
C6 Tc1 C5 36.73(13) . . ?
C1 Tc1 C5 114.14(15) 3_646 . ?
C1 Tc1 C5 65.86(15) . . ?
C6 Tc1 C5 36.73(13) 3_646 3_646 ?
C6 Tc1 C5 143.27(13) . 3_646 ?
C1 Tc1 C5 65.86(15) 3_646 3_646 ?
C1 Tc1 C5 114.14(15) . 3_646 ?
C5 Tc1 C5 180.00(12) . 3_646 ?
C6 Tc1 C3 78.63(15) 3_646 3_646 ?
C6 Tc1 C3 101.37(15) . 3_646 ?
C1 Tc1 C3 65.80(15) 3_646 3_646 ?
C1 Tc1 C3 114.20(15) . 3_646 ?
C5 Tc1 C3 113.67(14) . 3_646 ?
C5 Tc1 C3 66.33(14) 3_646 3_646 ?
C6 Tc1 C3 101.37(15) 3_646 . ?
C6 Tc1 C3 78.63(15) . . ?
C1 Tc1 C3 114.20(15) 3_646 . ?
C1 Tc1 C3 65.80(15) . . ?
C5 Tc1 C3 66.33(14) . . ?
C5 Tc1 C3 113.67(14) 3_646 . ?
C3 Tc1 C3 180.0 3_646 . ?
C6 Tc1 C4 66.25(15) 3_646 3_646 ?
C6 Tc1 C4 113.75(15) . 3_646 ?
C1 Tc1 C4 77.70(15) 3_646 3_646 ?
C1 Tc1 C4 102.30(15) . 3_646 ?
C5 Tc1 C4 143.41(14) . 3_646 ?
C5 Tc1 C4 36.59(14) 3_646 3_646 ?
C3 Tc1 C4 37.04(13) 3_646 3_646 ?
C3 Tc1 C4 142.96(13) . 3_646 ?
C6 Tc1 C4 113.75(15) 3_646 . ?
C6 Tc1 C4 66.25(15) . . ?
C1 Tc1 C4 102.30(15) 3_646 . ?
C1 Tc1 C4 77.70(15) . . ?
C5 Tc1 C4 36.59(14) . . ?
C5 Tc1 C4 143.41(14) 3_646 . ?
C3 Tc1 C4 142.96(13) 3_646 . ?
C3 Tc1 C4 37.04(13) . . ?
C4 Tc1 C4 180.0 3_646 . ?
C6 Tc1 C2 66.44(15) 3_646 3_646 ?
C6 Tc1 C2 113.56(15) . 3_646 ?
C1 Tc1 C2 36.23(15) 3_646 3_646 ?
C1 Tc1 C2 143.77(15) . 3_646 ?
C5 Tc1 C2 101.75(14) . 3_646 ?
C5 Tc1 C2 78.25(14) 3_646 3_646 ?
C3 Tc1 C2 37.04(14) 3_646 3_646 ?
C3 Tc1 C2 142.96(14) . 3_646 ?
C4 Tc1 C2 66.54(15) 3_646 3_646 ?
C4 Tc1 C2 113.46(15) . 3_646 ?
C6 Tc1 C2 113.56(15) 3_646 . ?
C6 Tc1 C2 66.44(15) . . ?
C1 Tc1 C2 143.77(15) 3_646 . ?
C1 Tc1 C2 36.23(15) . . ?
C5 Tc1 C2 78.25(14) . . ?
C5 Tc1 C2 101.75(14) 3_646 . ?
C3 Tc1 C2 142.96(14) 3_646 . ?
C3 Tc1 C2 37.04(14) . . ?
C4 Tc1 C2 113.46(15) 3_646 . ?
C4 Tc1 C2 66.54(15) . . ?
C2 Tc1 C2 180.00(19) 3_646 . ?
C12A Tc2 C12A 180.0 3 . ?
C12A Tc2 C11A 36.1(3) 3 3 ?
C12A Tc2 C11A 143.9(3) . 3 ?
C12A Tc2 C11A 143.9(3) 3 . ?
C12A Tc2 C11A 36.1(3) . . ?
C11A Tc2 C11A 180.0 3 . ?
C12A Tc2 C16A 115.3(3) 3 . ?
C12A Tc2 C16A 64.7(3) . . ?
C11A Tc2 C16A 144.0(3) 3 . ?
C11A Tc2 C16A 36.0(3) . . ?
C12A Tc2 C16A 64.7(3) 3 3 ?
C12A Tc2 C16A 115.3(3) . 3 ?
C11A Tc2 C16A 36.0(3) 3 3 ?
C11A Tc2 C16A 144.0(3) . 3 ?
C16A Tc2 C16A 180.0 . 3 ?
C12A Tc2 C15A 102.3(3) 3 . ?
C12A Tc2 C15A 77.7(3) . . ?
C11A Tc2 C15A 113.7(3) 3 . ?
C11A Tc2 C15A 66.3(3) . . ?
C16A Tc2 C15A 37.3(2) . . ?
C16A Tc2 C15A 142.7(2) 3 . ?
C12A Tc2 C15A 77.7(3) 3 3 ?
C12A Tc2 C15A 102.3(3) . 3 ?
C11A Tc2 C15A 66.3(3) 3 3 ?
C11A Tc2 C15A 113.7(3) . 3 ?
C16A Tc2 C15A 142.7(2) . 3 ?
C16A Tc2 C15A 37.3(2) 3 3 ?
C15A Tc2 C15A 180.0 . 3 ?
C12A Tc2 C13A 143.7(3) 3 . ?
C12A Tc2 C13A 36.3(3) . . ?
C11A Tc2 C13A 114.9(3) 3 . ?
C11A Tc2 C13A 65.1(3) . . ?
C16A Tc2 C13A 76.6(2) . . ?
C16A Tc2 C13A 103.4(2) 3 . ?
C15A Tc2 C13A 65.5(3) . . ?
C15A Tc2 C13A 114.5(3) 3 . ?
C12A Tc2 C13A 36.3(3) 3 3 ?
C12A Tc2 C13A 143.7(3) . 3 ?
C11A Tc2 C13A 65.1(3) 3 3 ?
C11A Tc2 C13A 114.9(3) . 3 ?
C16A Tc2 C13A 103.4(2) . 3 ?
C16A Tc2 C13A 76.6(2) 3 3 ?
C15A Tc2 C13A 114.5(3) . 3 ?
C15A Tc2 C13A 65.5(3) 3 3 ?
C13A Tc2 C13A 180.0 . 3 ?
C12A Tc2 C14A 65.9(3) 3 3 ?
C12A Tc2 C14A 114.1(3) . 3 ?
C11A Tc2 C14A 78.1(3) 3 3 ?
C11A Tc2 C14A 101.9(3) . 3 ?
C16A Tc2 C14A 113.7(2) . 3 ?
C16A Tc2 C14A 66.3(2) 3 3 ?
C15A Tc2 C14A 143.1(2) . 3 ?
C15A Tc2 C14A 36.9(2) 3 3 ?
C13A Tc2 C14A 143.6(3) . 3 ?
C13A Tc2 C14A 36.4(3) 3 3 ?
C12A Tc2 C14A 114.1(3) 3 . ?
C12A Tc2 C14A 65.9(3) . . ?
C11A Tc2 C14A 101.9(3) 3 . ?
C11A Tc2 C14A 78.1(3) . . ?
C16A Tc2 C14A 66.3(2) . . ?
C16A Tc2 C14A 113.7(2) 3 . ?
C15A Tc2 C14A 36.9(2) . . ?
C15A Tc2 C14A 143.1(2) 3 . ?
C13A Tc2 C14A 36.4(3) . . ?
C13A Tc2 C14A 143.6(3) 3 . ?
C14A Tc2 C14A 180.0 3 . ?
C2 C1 C6 121.6(4) . . ?
C2 C1 Tc1 72.2(2) . . ?
C6 C1 Tc1 71.26(19) . . ?
C2 C1 H1A 119.2 . . ?
C6 C1 H1A 119.2 . . ?
Tc1 C1 H1A 130.0 . . ?
C1 C2 C3 119.2(4) . . ?
C1 C2 Tc1 71.6(2) . . ?
C3 C2 Tc1 71.09(19) . . ?
C1 C2 H2A 120.4 . . ?
C3 C2 H2A 120.4 . . ?
Tc1 C2 H2A 129.2 . . ?
C4 C3 C2 119.7(4) . . ?
C4 C3 Tc1 71.59(19) . . ?
C2 C3 Tc1 71.9(2) . . ?
C4 C3 H3A 120.1 . . ?
C2 C3 H3A 120.1 . . ?
Tc1 C3 H3A 128.6 . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 Tc1 71.67(19) . . ?
C3 C4 Tc1 71.37(19) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
Tc1 C4 H4A 129.3 . . ?
C6 C5 C4 120.5(4) . . ?
C6 C5 Tc1 71.40(19) . . ?
C4 C5 Tc1 71.74(19) . . ?
C6 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
Tc1 C5 H5A 129.6 . . ?
C1 C6 C5 119.0(4) . . ?
C1 C6 Tc1 71.79(19) . . ?
C5 C6 Tc1 71.87(19) . . ?
C1 C6 H6A 120.5 . . ?
C5 C6 H6A 120.5 . . ?
Tc1 C6 H6A 127.9 . . ?
C12A C11A C16A 119.9(7) . . ?
C12A C11A Tc2 71.9(3) . . ?
C16A C11A Tc2 72.2(3) . . ?
C12A C11A H11A 120.0 . . ?
C16A C11A H11A 120.0 . . ?
Tc2 C11A H11A 128.0 . . ?
C13A C12A C11A 120.6(8) . . ?
C13A C12A Tc2 72.6(3) . . ?
C11A C12A Tc2 72.1(3) . . ?
C13A C12A H12A 119.7 . . ?
C11A C12A H12A 119.7 . . ?
Tc2 C12A H12A 127.8 . . ?
C12A C13A C14A 121.1(6) . . ?
C12A C13A Tc2 71.1(3) . . ?
C14A C13A Tc2 71.9(3) . . ?
C12A C13A H13A 119.4 . . ?
C14A C13A H13A 119.4 . . ?
Tc2 C13A H13A 130.2 . . ?
C13A C14A C15A 118.4(6) . . ?
C13A C14A Tc2 71.7(3) . . ?
C15A C14A Tc2 70.9(3) . . ?
C13A C14A H14A 120.8 . . ?
C15A C14A H14A 120.8 . . ?
Tc2 C14A H14A 128.7 . . ?
C14A C15A C16A 119.1(7) . . ?
C14A C15A Tc2 72.2(3) . . ?
C16A C15A Tc2 71.5(3) . . ?
C14A C15A H15A 120.4 . . ?
C16A C15A H15A 120.4 . . ?
Tc2 C15A H15A 127.9 . . ?
C11A C16A C15A 120.7(6) . . ?
C11A C16A Tc2 71.8(3) . . ?
C15A C16A Tc2 71.2(3) . . ?
C11A C16A H16A 119.7 . . ?
C15A C16A H16A 119.7 . . ?
Tc2 C16A H16A 129.9 . . ?
F2 P1 F3 91.03(16) . . ?
F2 P1 F4 90.68(15) . . ?
F3 P1 F4 91.03(15) . . ?
F2 P1 F6 89.58(15) . . ?
F3 P1 F6 179.05(15) . . ?
F4 P1 F6 89.70(14) . . ?
F2 P1 F5 178.67(18) . . ?
F3 P1 F5 90.02(15) . . ?
F4 P1 F5 90.13(15) . . ?
F6 P1 F5 89.37(15) . . ?
F2 P1 F1 90.50(15) . . ?
F3 P1 F1 89.88(14) . . ?
F4 P1 F1 178.50(15) . . ?
F6 P1 F1 89.38(14) . . ?
F5 P1 F1 88.68(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 Tc1 C1 C2 -46.4(4) 3_646 . . . ?
C6 Tc1 C1 C2 133.6(4) . . . . ?
C1 Tc1 C1 C2 38(7) 3_646 . . . ?
C5 Tc1 C1 C2 103.5(3) . . . . ?
C5 Tc1 C1 C2 -76.5(3) 3_646 . . . ?
C3 Tc1 C1 C2 -150.2(2) 3_646 . . . ?
C3 Tc1 C1 C2 29.8(2) . . . . ?
C4 Tc1 C1 C2 -113.1(3) 3_646 . . . ?
C4 Tc1 C1 C2 66.9(3) . . . . ?
C2 Tc1 C1 C2 180.000(1) 3_646 . . . ?
C6 Tc1 C1 C6 180.0 3_646 . . . ?
C1 Tc1 C1 C6 -96(7) 3_646 . . . ?
C5 Tc1 C1 C6 -30.1(2) . . . . ?
C5 Tc1 C1 C6 149.9(2) 3_646 . . . ?
C3 Tc1 C1 C6 76.2(3) 3_646 . . . ?
C3 Tc1 C1 C6 -103.8(3) . . . . ?
C4 Tc1 C1 C6 113.3(3) 3_646 . . . ?
C4 Tc1 C1 C6 -66.7(3) . . . . ?
C2 Tc1 C1 C6 46.4(4) 3_646 . . . ?
C2 Tc1 C1 C6 -133.6(4) . . . . ?
C6 C1 C2 C3 -1.2(5) . . . . ?
Tc1 C1 C2 C3 -54.8(3) . . . . ?
C6 C1 C2 Tc1 53.6(3) . . . . ?
C6 Tc1 C2 C1 151.7(2) 3_646 . . . ?
C6 Tc1 C2 C1 -28.3(2) . . . . ?
C1 Tc1 C2 C1 180.0 3_646 . . . ?
C5 Tc1 C2 C1 -65.0(3) . . . . ?
C5 Tc1 C2 C1 115.0(3) 3_646 . . . ?
C3 Tc1 C2 C1 48.9(4) 3_646 . . . ?
C3 Tc1 C2 C1 -131.1(4) . . . . ?
C4 Tc1 C2 C1 78.5(3) 3_646 . . . ?
C4 Tc1 C2 C1 -101.5(3) . . . . ?
C2 Tc1 C2 C1 81(9) 3_646 . . . ?
C6 Tc1 C2 C3 -77.3(3) 3_646 . . . ?
C6 Tc1 C2 C3 102.7(3) . . . . ?
C1 Tc1 C2 C3 -48.9(4) 3_646 . . . ?
C1 Tc1 C2 C3 131.1(4) . . . . ?
C5 Tc1 C2 C3 66.1(2) . . . . ?
C5 Tc1 C2 C3 -113.9(2) 3_646 . . . ?
C3 Tc1 C2 C3 180.0 3_646 . . . ?
C4 Tc1 C2 C3 -150.4(2) 3_646 . . . ?
C4 Tc1 C2 C3 29.6(2) . . . . ?
C2 Tc1 C2 C3 -147(8) 3_646 . . . ?
C1 C2 C3 C4 -0.3(5) . . . . ?
Tc1 C2 C3 C4 -55.3(3) . . . . ?
C1 C2 C3 Tc1 55.0(3) . . . . ?
C6 Tc1 C3 C4 -114.6(2) 3_646 . . . ?
C6 Tc1 C3 C4 65.4(2) . . . . ?
C1 Tc1 C3 C4 -78.0(3) 3_646 . . . ?
C1 Tc1 C3 C4 102.0(3) . . . . ?
C5 Tc1 C3 C4 29.0(2) . . . . ?
C5 Tc1 C3 C4 -151.0(2) 3_646 . . . ?
C3 Tc1 C3 C4 141(15) 3_646 . . . ?
C4 Tc1 C3 C4 180.0 3_646 . . . ?
C2 Tc1 C3 C4 -48.8(4) 3_646 . . . ?
C2 Tc1 C3 C4 131.2(4) . . . . ?
C6 Tc1 C3 C2 114.2(2) 3_646 . . . ?
C6 Tc1 C3 C2 -65.8(2) . . . . ?
C1 Tc1 C3 C2 150.8(2) 3_646 . . . ?
C1 Tc1 C3 C2 -29.2(2) . . . . ?
C5 Tc1 C3 C2 -102.2(3) . . . . ?
C5 Tc1 C3 C2 77.8(3) 3_646 . . . ?
C3 Tc1 C3 C2 9(15) 3_646 . . . ?
C4 Tc1 C3 C2 48.8(4) 3_646 . . . ?
C4 Tc1 C3 C2 -131.2(4) . . . . ?
C2 Tc1 C3 C2 180.0 3_646 . . . ?
C2 C3 C4 C5 0.7(5) . . . . ?
Tc1 C3 C4 C5 -54.7(3) . . . . ?
C2 C3 C4 Tc1 55.4(3) . . . . ?
C6 Tc1 C4 C5 -151.2(2) 3_646 . . . ?
C6 Tc1 C4 C5 28.8(2) . . . . ?
C1 Tc1 C4 C5 -114.1(2) 3_646 . . . ?
C1 Tc1 C4 C5 65.9(2) . . . . ?
C5 Tc1 C4 C5 180.0 3_646 . . . ?
C3 Tc1 C4 C5 -48.2(4) 3_646 . . . ?
C3 Tc1 C4 C5 131.8(4) . . . . ?
C4 Tc1 C4 C5 108(21) 3_646 . . . ?
C2 Tc1 C4 C5 -77.7(3) 3_646 . . . ?
C2 Tc1 C4 C5 102.3(3) . . . . ?
C6 Tc1 C4 C3 77.0(3) 3_646 . . . ?
C6 Tc1 C4 C3 -103.0(3) . . . . ?
C1 Tc1 C4 C3 114.1(2) 3_646 . . . ?
C1 Tc1 C4 C3 -65.9(2) . . . . ?
C5 Tc1 C4 C3 -131.8(4) . . . . ?
C5 Tc1 C4 C3 48.2(4) 3_646 . . . ?
C3 Tc1 C4 C3 180.0 3_646 . . . ?
C4 Tc1 C4 C3 -24(21) 3_646 . . . ?
C2 Tc1 C4 C3 150.4(2) 3_646 . . . ?
C2 Tc1 C4 C3 -29.6(2) . . . . ?
C3 C4 C5 C6 0.3(5) . . . . ?
Tc1 C4 C5 C6 -54.2(3) . . . . ?
C3 C4 C5 Tc1 54.6(3) . . . . ?
C6 Tc1 C5 C6 180.0 3_646 . . . ?
C1 Tc1 C5 C6 -149.8(2) 3_646 . . . ?
C1 Tc1 C5 C6 30.2(2) . . . . ?
C5 Tc1 C5 C6 103(55) 3_646 . . . ?
C3 Tc1 C5 C6 -76.9(3) 3_646 . . . ?
C3 Tc1 C5 C6 103.1(3) . . . . ?
C4 Tc1 C5 C6 -47.5(4) 3_646 . . . ?
C4 Tc1 C5 C6 132.5(4) . . . . ?
C2 Tc1 C5 C6 -113.8(2) 3_646 . . . ?
C2 Tc1 C5 C6 66.2(2) . . . . ?
C6 Tc1 C5 C4 47.5(4) 3_646 . . . ?
C6 Tc1 C5 C4 -132.5(4) . . . . ?
C1 Tc1 C5 C4 77.8(3) 3_646 . . . ?
C1 Tc1 C5 C4 -102.2(3) . . . . ?
C5 Tc1 C5 C4 -29(55) 3_646 . . . ?
C3 Tc1 C5 C4 150.7(2) 3_646 . . . ?
C3 Tc1 C5 C4 -29.3(2) . . . . ?
C4 Tc1 C5 C4 180.0 3_646 . . . ?
C2 Tc1 C5 C4 113.7(2) 3_646 . . . ?
C2 Tc1 C5 C4 -66.3(2) . . . . ?
C2 C1 C6 C5 2.2(5) . . . . ?
Tc1 C1 C6 C5 56.2(3) . . . . ?
C2 C1 C6 Tc1 -54.0(3) . . . . ?
C4 C5 C6 C1 -1.7(5) . . . . ?
Tc1 C5 C6 C1 -56.1(3) . . . . ?
C4 C5 C6 Tc1 54.4(3) . . . . ?
C6 Tc1 C6 C1 176(12) 3_646 . . . ?
C1 Tc1 C6 C1 180.0 3_646 . . . ?
C5 Tc1 C6 C1 130.1(4) . . . . ?
C5 Tc1 C6 C1 -49.9(4) 3_646 . . . ?
C3 Tc1 C6 C1 -115.4(3) 3_646 . . . ?
C3 Tc1 C6 C1 64.6(3) . . . . ?
C4 Tc1 C6 C1 -78.6(3) 3_646 . . . ?
C4 Tc1 C6 C1 101.4(3) . . . . ?
C2 Tc1 C6 C1 -152.2(2) 3_646 . . . ?
C2 Tc1 C6 C1 27.8(2) . . . . ?
C6 Tc1 C6 C5 46(12) 3_646 . . . ?
C1 Tc1 C6 C5 49.9(4) 3_646 . . . ?
C1 Tc1 C6 C5 -130.1(4) . . . . ?
C5 Tc1 C6 C5 180.0 3_646 . . . ?
C3 Tc1 C6 C5 114.5(2) 3_646 . . . ?
C3 Tc1 C6 C5 -65.5(2) . . . . ?
C4 Tc1 C6 C5 151.3(2) 3_646 . . . ?
C4 Tc1 C6 C5 -28.7(2) . . . . ?
C2 Tc1 C6 C5 77.7(3) 3_646 . . . ?
C2 Tc1 C6 C5 -102.3(3) . . . . ?
C12A Tc2 C11A C12A 180.0 3 . . . ?
C11A Tc2 C11A C12A 75(5) 3 . . . ?
C16A Tc2 C11A C12A -131.0(7) . . . . ?
C16A Tc2 C11A C12A 49.0(7) 3 . . . ?
C15A Tc2 C11A C12A -102.0(5) . . . . ?
C15A Tc2 C11A C12A 78.0(5) 3 . . . ?
C13A Tc2 C11A C12A -29.2(5) . . . . ?
C13A Tc2 C11A C12A 150.8(5) 3 . . . ?
C14A Tc2 C11A C12A 114.8(6) 3 . . . ?
C14A Tc2 C11A C12A -65.2(6) . . . . ?
C12A Tc2 C11A C16A -49.0(7) 3 . . . ?
C12A Tc2 C11A C16A 131.0(7) . . . . ?
C11A Tc2 C11A C16A -154(5) 3 . . . ?
C16A Tc2 C11A C16A 180.0 3 . . . ?
C15A Tc2 C11A C16A 29.0(4) . . . . ?
C15A Tc2 C11A C16A -151.0(4) 3 . . . ?
C13A Tc2 C11A C16A 101.8(5) . . . . ?
C13A Tc2 C11A C16A -78.2(5) 3 . . . ?
C14A Tc2 C11A C16A -114.2(5) 3 . . . ?
C14A Tc2 C11A C16A 65.8(5) . . . . ?
C16A C11A C12A C13A 0.1(10) . . . . ?
Tc2 C11A C12A C13A 56.1(6) . . . . ?
C16A C11A C12A Tc2 -56.0(6) . . . . ?
C12A Tc2 C12A C13A 50.3(4) 3 . . . ?
C11A Tc2 C12A C13A 48.5(8) 3 . . . ?
C11A Tc2 C12A C13A -131.5(8) . . . . ?
C16A Tc2 C12A C13A -102.2(5) . . . . ?
C16A Tc2 C12A C13A 77.8(5) 3 . . . ?
C15A Tc2 C12A C13A -65.1(5) . . . . ?
C15A Tc2 C12A C13A 114.9(5) 3 . . . ?
C13A Tc2 C12A C13A 180.0 3 . . . ?
C14A Tc2 C12A C13A 151.8(4) 3 . . . ?
C14A Tc2 C12A C13A -28.2(4) . . . . ?
C12A Tc2 C12A C11A -178.2(6) 3 . . . ?
C11A Tc2 C12A C11A 180.0 3 . . . ?
C16A Tc2 C12A C11A 29.4(5) . . . . ?
C16A Tc2 C12A C11A -150.6(5) 3 . . . ?
C15A Tc2 C12A C11A 66.4(5) . . . . ?
C15A Tc2 C12A C11A -113.6(5) 3 . . . ?
C13A Tc2 C12A C11A 131.5(8) . . . . ?
C13A Tc2 C12A C11A -48.5(8) 3 . . . ?
C14A Tc2 C12A C11A -76.7(6) 3 . . . ?
C14A Tc2 C12A C11A 103.3(6) . . . . ?
C11A C12A C13A C14A -2.1(10) . . . . ?
Tc2 C12A C13A C14A 53.8(5) . . . . ?
C11A C12A C13A Tc2 -55.9(6) . . . . ?
C12A Tc2 C13A C12A 180.0 3 . . . ?
C11A Tc2 C13A C12A -150.9(5) 3 . . . ?
C11A Tc2 C13A C12A 29.1(5) . . . . ?
C16A Tc2 C13A C12A 65.3(5) . . . . ?
C16A Tc2 C13A C12A -114.7(5) 3 . . . ?
C15A Tc2 C13A C12A 103.1(5) . . . . ?
C15A Tc2 C13A C12A -76.9(5) 3 . . . ?
C13A Tc2 C13A C12A 88(7) 3 . . . ?
C14A Tc2 C13A C12A -46.6(7) 3 . . . ?
C14A Tc2 C13A C12A 133.4(7) . . . . ?
C12A Tc2 C13A C14A 46.6(7) 3 . . . ?
C12A Tc2 C13A C14A -133.4(7) . . . . ?
C11A Tc2 C13A C14A 75.7(5) 3 . . . ?
C11A Tc2 C13A C14A -104.3(5) . . . . ?
C16A Tc2 C13A C14A -68.1(4) . . . . ?
C16A Tc2 C13A C14A 111.9(4) 3 . . . ?
C15A Tc2 C13A C14A -30.3(4) . . . . ?
C15A Tc2 C13A C14A 149.7(4) 3 . . . ?
C13A Tc2 C13A C14A -45(7) 3 . . . ?
C14A Tc2 C13A C14A 180.0 3 . . . ?
C12A C13A C14A C15A 1.8(9) . . . . ?
Tc2 C13A C14A C15A 55.3(5) . . . . ?
C12A C13A C14A Tc2 -53.5(5) . . . . ?
C12A Tc2 C14A C13A -151.9(4) 3 . . . ?
C12A Tc2 C14A C13A 28.1(4) . . . . ?
C11A Tc2 C14A C13A -116.1(4) 3 . . . ?
C11A Tc2 C14A C13A 63.9(4) . . . . ?
C16A Tc2 C14A C13A 99.8(5) . . . . ?
C16A Tc2 C14A C13A -80.2(5) 3 . . . ?
C15A Tc2 C14A C13A 130.1(6) . . . . ?
C15A Tc2 C14A C13A -49.9(6) 3 . . . ?
C13A Tc2 C14A C13A 180.0 3 . . . ?
C14A Tc2 C14A C13A 93(2) 3 . . . ?
C12A Tc2 C14A C15A 78.0(5) 3 . . . ?
C12A Tc2 C14A C15A -102.0(5) . . . . ?
C11A Tc2 C14A C15A 113.8(5) 3 . . . ?
C11A Tc2 C14A C15A -66.2(5) . . . . ?
C16A Tc2 C14A C15A -30.3(5) . . . . ?
C16A Tc2 C14A C15A 149.7(5) 3 . . . ?
C15A Tc2 C14A C15A 180.0 3 . . . ?
C13A Tc2 C14A C15A -130.1(6) . . . . ?
C13A Tc2 C14A C15A 49.9(6) 3 . . . ?
C14A Tc2 C14A C15A -37(2) 3 . . . ?
C13A C14A C15A C16A 0.3(9) . . . . ?
Tc2 C14A C15A C16A 56.0(5) . . . . ?
C13A C14A C15A Tc2 -55.7(5) . . . . ?
C12A Tc2 C15A C14A -113.9(5) 3 . . . ?
C12A Tc2 C15A C14A 66.1(5) . . . . ?
C11A Tc2 C15A C14A -77.8(5) 3 . . . ?
C11A Tc2 C15A C14A 102.2(5) . . . . ?
C16A Tc2 C15A C14A 130.3(7) . . . . ?
C16A Tc2 C15A C14A -49.7(7) 3 . . . ?
C15A Tc2 C15A C14A -160.9(12) 3 . . . ?
C13A Tc2 C15A C14A 29.9(4) . . . . ?
C13A Tc2 C15A C14A -150.1(4) 3 . . . ?
C14A Tc2 C15A C14A 180.0 3 . . . ?
C12A Tc2 C15A C16A 115.8(5) 3 . . . ?
C12A Tc2 C15A C16A -64.2(5) . . . . ?
C11A Tc2 C15A C16A 151.9(4) 3 . . . ?
C11A Tc2 C15A C16A -28.1(4) . . . . ?
C16A Tc2 C15A C16A 180.000(2) 3 . . . ?
C15A Tc2 C15A C16A 68.8(13) 3 . . . ?
C13A Tc2 C15A C16A -100.3(5) . . . . ?
C13A Tc2 C15A C16A 79.7(5) 3 . . . ?
C14A Tc2 C15A C16A 49.7(7) 3 . . . ?
C14A Tc2 C15A C16A -130.3(7) . . . . ?
C12A C11A C16A C15A 2.0(10) . . . . ?
Tc2 C11A C16A C15A -53.8(6) . . . . ?
C12A C11A C16A Tc2 55.8(6) . . . . ?
C14A C15A C16A C11A -2.2(10) . . . . ?
Tc2 C15A C16A C11A 54.1(6) . . . . ?
C14A C15A C16A Tc2 -56.3(5) . . . . ?
C12A Tc2 C16A C11A 150.6(5) 3 . . . ?
C12A Tc2 C16A C11A -29.4(5) . . . . ?
C11A Tc2 C16A C11A 180.0 3 . . . ?
C16A Tc2 C16A C11A 50(3) 3 . . . ?
C15A Tc2 C16A C11A -132.8(7) . . . . ?
C15A Tc2 C16A C11A 47.2(7) 3 . . . ?
C13A Tc2 C16A C11A -65.9(5) . . . . ?
C13A Tc2 C16A C11A 114.1(5) 3 . . . ?
C14A Tc2 C16A C11A 77.2(5) 3 . . . ?
C14A Tc2 C16A C11A -102.8(5) . . . . ?
C12A Tc2 C16A C15A -76.6(5) 3 . . . ?
C12A Tc2 C16A C15A 103.4(5) . . . . ?
C11A Tc2 C16A C15A -47.2(7) 3 . . . ?
C11A Tc2 C16A C15A 132.8(7) . . . . ?
C16A Tc2 C16A C15A -177(3) 3 . . . ?
C15A Tc2 C16A C15A 180.0 3 . . . ?
C13A Tc2 C16A C15A 66.9(5) . . . . ?
C13A Tc2 C16A C15A -113.1(5) 3 . . . ?
C14A Tc2 C16A C15A -150.0(5) 3 . . . ?
C14A Tc2 C16A C15A 30.0(5) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.104
_database_code_depnum_ccdc_archive 'CCDC 1017765'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_meb211113

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Tc(toluene)2]PF6'
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H16 Tc, F6 P '
_chemical_formula_sum            'C14 H16 F6 P Tc'
_chemical_formula_weight         427.24

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'
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'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   7.7559(8)
_cell_length_b                   11.0030(8)
_cell_length_c                   8.9353(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.474(9)
_cell_angle_gamma                90.00
_cell_volume                     754.20(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    1610
_cell_measurement_theta_min      2.9280
_cell_measurement_theta_max      29.2960

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_T_max  0.9062
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 none 
;

_diffrn_ambient_temperature      183(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  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5202
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         26.37
_reflns_number_total             1545
_reflns_number_gt                1125
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0403P)²+0.0475P] where P=(Fo²+2Fc²)/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         1545
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Tc1 Tc 0.0000 0.0000 0.0000 0.02749(18) Uani 1 2 d S . .
C1 C -0.0924(5) -0.0706(3) 0.2102(4) 0.0346(9) Uani 1 1 d . . .
C2 C -0.2087(5) -0.1084(4) 0.0822(4) 0.0380(10) Uani 1 1 d . . .
H2A H -0.2343 -0.1925 0.0688 0.046 Uiso 1 1 calc R . .
C3 C -0.2875(6) -0.0254(4) -0.0258(5) 0.0420(11) Uani 1 1 d . . .
H3A H -0.3658 -0.0533 -0.1107 0.050 Uiso 1 1 calc R . .
C4 C -0.2505(6) 0.0989(4) -0.0083(5) 0.0413(11) Uani 1 1 d . . .
H4A H -0.3022 0.1554 -0.0819 0.050 Uiso 1 1 calc R . .
C5 C -0.1376(6) 0.1390(3) 0.1177(5) 0.0385(10) Uani 1 1 d . . .
H5A H -0.1138 0.2234 0.1304 0.046 Uiso 1 1 calc R . .
C6 C -0.0585(6) 0.0563(3) 0.2261(4) 0.0366(10) Uani 1 1 d . . .
H6A H 0.0186 0.0853 0.3111 0.044 Uiso 1 1 calc R . .
C7 C -0.0088(6) -0.1595(4) 0.3248(4) 0.0489(12) Uani 1 1 d . . .
H7C H -0.0833 -0.1709 0.4033 0.059 Uiso 1 1 calc R . .
H7B H 0.1051 -0.1283 0.3710 0.059 Uiso 1 1 calc R . .
H7A H 0.0065 -0.2374 0.2754 0.059 Uiso 1 1 calc R . .
P1 P 0.0000 0.5000 0.0000 0.0317(4) Uani 1 2 d S . .
F1 F 0.0487(4) 0.4156(2) 0.1438(3) 0.0702(9) Uani 1 1 d . . .
F2 F -0.1570(4) 0.4114(2) -0.0621(3) 0.0668(9) Uani 1 1 d . . .
F3 F -0.1244(4) 0.5765(3) 0.0879(4) 0.0888(11) Uani 1 1 d . . .


_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
Tc1 C5 2.217(4) 3 ?
Tc1 C5 2.217(4) . ?
Tc1 C4 2.219(4) . ?
Tc1 C4 2.219(4) 3 ?
Tc1 C2 2.221(4) . ?
Tc1 C2 2.221(4) 3 ?
Tc1 C6 2.223(4) . ?
Tc1 C6 2.223(4) 3 ?
Tc1 C3 2.225(4) . ?
Tc1 C3 2.225(4) 3 ?
Tc1 C1 2.245(4) . ?
Tc1 C1 2.245(4) 3 ?
C1 C2 1.411(6) . ?
C1 C6 1.424(5) . ?
C1 C7 1.493(5) . ?
C2 C3 1.402(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.401(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.393(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.403(6) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 H7C 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7A 0.9800 . ?
P1 F3 1.575(3) . ?
P1 F3 1.575(3) 3_565 ?
P1 F1 1.585(2) 3_565 ?
P1 F1 1.585(2) . ?
P1 F2 1.595(2) 3_565 ?
P1 F2 1.595(2) . ?

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
C5 Tc1 C5 179.999(1) 3 . ?
C5 Tc1 C4 143.41(15) 3 . ?
C5 Tc1 C4 36.59(15) . . ?
C5 Tc1 C4 36.59(15) 3 3 ?
C5 Tc1 C4 143.40(15) . 3 ?
C4 Tc1 C4 180.0 . 3 ?
C5 Tc1 C2 102.21(15) 3 . ?
C5 Tc1 C2 77.79(15) . . ?
C4 Tc1 C2 66.24(16) . . ?
C4 Tc1 C2 113.76(16) 3 . ?
C5 Tc1 C2 77.79(15) 3 3 ?
C5 Tc1 C2 102.21(15) . 3 ?
C4 Tc1 C2 113.76(16) . 3 ?
C4 Tc1 C2 66.24(16) 3 3 ?
C2 Tc1 C2 180.0 . 3 ?
C5 Tc1 C6 143.17(14) 3 . ?
C5 Tc1 C6 36.83(14) . . ?
C4 Tc1 C6 66.34(15) . . ?
C4 Tc1 C6 113.66(15) 3 . ?
C2 Tc1 C6 65.98(14) . . ?
C2 Tc1 C6 114.02(14) 3 . ?
C5 Tc1 C6 36.83(14) 3 3 ?
C5 Tc1 C6 143.17(14) . 3 ?
C4 Tc1 C6 113.66(15) . 3 ?
C4 Tc1 C6 66.34(15) 3 3 ?
C2 Tc1 C6 114.02(14) . 3 ?
C2 Tc1 C6 65.98(14) 3 3 ?
C6 Tc1 C6 180.0 . 3 ?
C5 Tc1 C3 114.15(15) 3 . ?
C5 Tc1 C3 65.85(15) . . ?
C4 Tc1 C3 36.76(14) . . ?
C4 Tc1 C3 143.24(14) 3 . ?
C2 Tc1 C3 36.76(15) . . ?
C2 Tc1 C3 143.24(15) 3 . ?
C6 Tc1 C3 78.09(16) . . ?
C6 Tc1 C3 101.91(16) 3 . ?
C5 Tc1 C3 65.85(15) 3 3 ?
C5 Tc1 C3 114.15(15) . 3 ?
C4 Tc1 C3 143.24(14) . 3 ?
C4 Tc1 C3 36.76(14) 3 3 ?
C2 Tc1 C3 143.24(15) . 3 ?
C2 Tc1 C3 36.76(15) 3 3 ?
C6 Tc1 C3 101.91(16) . 3 ?
C6 Tc1 C3 78.10(16) 3 3 ?
C3 Tc1 C3 180.0 . 3 ?
C5 Tc1 C1 113.16(13) 3 . ?
C5 Tc1 C1 66.84(13) . . ?
C4 Tc1 C1 79.16(15) . . ?
C4 Tc1 C1 100.84(15) 3 . ?
C2 Tc1 C1 36.83(14) . . ?
C2 Tc1 C1 143.17(14) 3 . ?
C6 Tc1 C1 37.18(15) . . ?
C6 Tc1 C1 142.82(15) 3 . ?
C3 Tc1 C1 66.72(15) . . ?
C3 Tc1 C1 113.27(15) 3 . ?
C5 Tc1 C1 66.84(13) 3 3 ?
C5 Tc1 C1 113.16(13) . 3 ?
C4 Tc1 C1 100.84(15) . 3 ?
C4 Tc1 C1 79.16(15) 3 3 ?
C2 Tc1 C1 143.17(14) . 3 ?
C2 Tc1 C1 36.83(14) 3 3 ?
C6 Tc1 C1 142.82(15) . 3 ?
C6 Tc1 C1 37.18(15) 3 3 ?
C3 Tc1 C1 113.28(15) . 3 ?
C3 Tc1 C1 66.73(15) 3 3 ?
C1 Tc1 C1 180.0 . 3 ?
C2 C1 C6 117.1(3) . . ?
C2 C1 C7 121.6(3) . . ?
C6 C1 C7 121.2(3) . . ?
C2 C1 Tc1 70.6(2) . . ?
C6 C1 Tc1 70.5(2) . . ?
C7 C1 Tc1 129.8(3) . . ?
C3 C2 C1 121.9(4) . . ?
C3 C2 Tc1 71.8(2) . . ?
C1 C2 Tc1 72.5(2) . . ?
C3 C2 H2A 119.1 . . ?
C1 C2 H2A 119.1 . . ?
Tc1 C2 H2A 129.1 . . ?
C4 C3 C2 119.9(4) . . ?
C4 C3 Tc1 71.4(2) . . ?
C2 C3 Tc1 71.4(2) . . ?
C4 C3 H3A 120.1 . . ?
C2 C3 H3A 120.1 . . ?
Tc1 C3 H3A 129.5 . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 Tc1 71.6(2) . . ?
C3 C4 Tc1 71.9(2) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
Tc1 C4 H4A 128.5 . . ?
C4 C5 C6 120.8(4) . . ?
C4 C5 Tc1 71.8(2) . . ?
C6 C5 Tc1 71.8(2) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
Tc1 C5 H5A 129.2 . . ?
C5 C6 C1 120.8(3) . . ?
C5 C6 Tc1 71.4(2) . . ?
C1 C6 Tc1 72.3(2) . . ?
C5 C6 H6A 119.6 . . ?
C1 C6 H6A 119.6 . . ?
Tc1 C6 H6A 129.2 . . ?
C1 C7 H7C 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7C C7 H7B 109.5 . . ?
C1 C7 H7A 109.5 . . ?
H7C C7 H7A 109.5 . . ?
H7B C7 H7A 109.5 . . ?
F3 P1 F3 180.0 . 3_565 ?
F3 P1 F1 90.03(17) . 3_565 ?
F3 P1 F1 89.97(17) 3_565 3_565 ?
F3 P1 F1 89.97(17) . . ?
F3 P1 F1 90.03(17) 3_565 . ?
F1 P1 F1 180.0 3_565 . ?
F3 P1 F2 89.57(17) . 3_565 ?
F3 P1 F2 90.43(17) 3_565 3_565 ?
F1 P1 F2 90.11(13) 3_565 3_565 ?
F1 P1 F2 89.89(13) . 3_565 ?
F3 P1 F2 90.43(17) . . ?
F3 P1 F2 89.57(17) 3_565 . ?
F1 P1 F2 89.89(13) 3_565 . ?
F1 P1 F2 90.11(13) . . ?
F2 P1 F2 180.0 3_565 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 Tc1 C1 C2 -79.2(3) 3 . . . ?
C5 Tc1 C1 C2 100.8(3) . . . . ?
C4 Tc1 C1 C2 64.6(3) . . . . ?
C4 Tc1 C1 C2 -115.4(3) 3 . . . ?
C2 Tc1 C1 C2 180.0 3 . . . ?
C6 Tc1 C1 C2 129.6(3) . . . . ?
C6 Tc1 C1 C2 -50.4(3) 3 . . . ?
C3 Tc1 C1 C2 28.3(2) . . . . ?
C3 Tc1 C1 C2 -151.7(2) 3 . . . ?
C1 Tc1 C1 C2 -37(4) 3 . . . ?
C5 Tc1 C1 C6 151.2(2) 3 . . . ?
C5 Tc1 C1 C6 -28.8(2) . . . . ?
C4 Tc1 C1 C6 -64.9(2) . . . . ?
C4 Tc1 C1 C6 115.1(2) 3 . . . ?
C2 Tc1 C1 C6 -129.6(3) . . . . ?
C2 Tc1 C1 C6 50.4(3) 3 . . . ?
C6 Tc1 C1 C6 180.0 3 . . . ?
C3 Tc1 C1 C6 -101.3(2) . . . . ?
C3 Tc1 C1 C6 78.7(2) 3 . . . ?
C1 Tc1 C1 C6 -167(4) 3 . . . ?
C5 Tc1 C1 C7 36.3(4) 3 . . . ?
C5 Tc1 C1 C7 -143.7(4) . . . . ?
C4 Tc1 C1 C7 -179.9(4) . . . . ?
C4 Tc1 C1 C7 0.1(4) 3 . . . ?
C2 Tc1 C1 C7 115.5(4) . . . . ?
C2 Tc1 C1 C7 -64.5(4) 3 . . . ?
C6 Tc1 C1 C7 -114.9(4) . . . . ?
C6 Tc1 C1 C7 65.1(4) 3 . . . ?
C3 Tc1 C1 C7 143.8(4) . . . . ?
C3 Tc1 C1 C7 -36.2(4) 3 . . . ?
C1 Tc1 C1 C7 79(4) 3 . . . ?
C6 C1 C2 C3 0.3(6) . . . . ?
C7 C1 C2 C3 180.0(4) . . . . ?
Tc1 C1 C2 C3 -54.5(4) . . . . ?
C6 C1 C2 Tc1 54.8(3) . . . . ?
C7 C1 C2 Tc1 -125.5(4) . . . . ?
C5 Tc1 C2 C3 -114.2(3) 3 . . . ?
C5 Tc1 C2 C3 65.8(3) . . . . ?
C4 Tc1 C2 C3 29.1(2) . . . . ?
C4 Tc1 C2 C3 -150.9(2) 3 . . . ?
C2 Tc1 C2 C3 136(10) 3 . . . ?
C6 Tc1 C2 C3 102.7(3) . . . . ?
C6 Tc1 C2 C3 -77.3(3) 3 . . . ?
C3 Tc1 C2 C3 180.0 3 . . . ?
C1 Tc1 C2 C3 133.3(4) . . . . ?
C1 Tc1 C2 C3 -46.7(4) 3 . . . ?
C5 Tc1 C2 C1 112.5(2) 3 . . . ?
C5 Tc1 C2 C1 -67.5(2) . . . . ?
C4 Tc1 C2 C1 -104.2(3) . . . . ?
C4 Tc1 C2 C1 75.8(3) 3 . . . ?
C2 Tc1 C2 C1 3(10) 3 . . . ?
C6 Tc1 C2 C1 -30.7(2) . . . . ?
C6 Tc1 C2 C1 149.3(2) 3 . . . ?
C3 Tc1 C2 C1 -133.3(4) . . . . ?
C3 Tc1 C2 C1 46.7(4) 3 . . . ?
C1 Tc1 C2 C1 180.0 3 . . . ?
C1 C2 C3 C4 0.3(7) . . . . ?
Tc1 C2 C3 C4 -54.5(4) . . . . ?
C1 C2 C3 Tc1 54.8(4) . . . . ?
C5 Tc1 C3 C4 -150.5(2) 3 . . . ?
C5 Tc1 C3 C4 29.5(2) . . . . ?
C4 Tc1 C3 C4 180.0 3 . . . ?
C2 Tc1 C3 C4 131.9(4) . . . . ?
C2 Tc1 C3 C4 -48.1(4) 3 . . . ?
C6 Tc1 C3 C4 66.2(3) . . . . ?
C6 Tc1 C3 C4 -113.8(3) 3 . . . ?
C3 Tc1 C3 C4 147.6(10) 3 . . . ?
C1 Tc1 C3 C4 103.5(3) . . . . ?
C1 Tc1 C3 C4 -76.5(3) 3 . . . ?
C5 Tc1 C3 C2 77.7(3) 3 . . . ?
C5 Tc1 C3 C2 -102.3(3) . . . . ?
C4 Tc1 C3 C2 -131.9(4) . . . . ?
C4 Tc1 C3 C2 48.1(4) 3 . . . ?
C2 Tc1 C3 C2 180.0 3 . . . ?
C6 Tc1 C3 C2 -65.6(2) . . . . ?
C6 Tc1 C3 C2 114.4(2) 3 . . . ?
C3 Tc1 C3 C2 15.7(10) 3 . . . ?
C1 Tc1 C3 C2 -28.3(2) . . . . ?
C1 Tc1 C3 C2 151.7(2) 3 . . . ?
C2 C3 C4 C5 -0.9(6) . . . . ?
Tc1 C3 C4 C5 -55.4(4) . . . . ?
C2 C3 C4 Tc1 54.5(4) . . . . ?
C5 Tc1 C4 C5 180.0 3 . . . ?
C4 Tc1 C4 C5 -29(3) 3 . . . ?
C2 Tc1 C4 C5 101.8(3) . . . . ?
C2 Tc1 C4 C5 -78.2(3) 3 . . . ?
C6 Tc1 C4 C5 28.9(2) . . . . ?
C6 Tc1 C4 C5 -151.1(2) 3 . . . ?
C3 Tc1 C4 C5 131.0(4) . . . . ?
C3 Tc1 C4 C5 -49.0(4) 3 . . . ?
C1 Tc1 C4 C5 65.6(2) . . . . ?
C1 Tc1 C4 C5 -114.4(2) 3 . . . ?
C5 Tc1 C4 C3 49.0(4) 3 . . . ?
C5 Tc1 C4 C3 -131.0(4) . . . . ?
C4 Tc1 C4 C3 -160(3) 3 . . . ?
C2 Tc1 C4 C3 -29.1(2) . . . . ?
C2 Tc1 C4 C3 150.9(2) 3 . . . ?
C6 Tc1 C4 C3 -102.1(3) . . . . ?
C6 Tc1 C4 C3 77.9(3) 3 . . . ?
C3 Tc1 C4 C3 180.0 3 . . . ?
C1 Tc1 C4 C3 -65.4(3) . . . . ?
C1 Tc1 C4 C3 114.6(3) 3 . . . ?
C3 C4 C5 C6 0.9(6) . . . . ?
Tc1 C4 C5 C6 -54.6(4) . . . . ?
C3 C4 C5 Tc1 55.6(4) . . . . ?
C5 Tc1 C5 C4 120(5) 3 . . . ?
C4 Tc1 C5 C4 180.0 3 . . . ?
C2 Tc1 C5 C4 -66.4(3) . . . . ?
C2 Tc1 C5 C4 113.6(3) 3 . . . ?
C6 Tc1 C5 C4 -132.5(4) . . . . ?
C6 Tc1 C5 C4 47.5(4) 3 . . . ?
C3 Tc1 C5 C4 -29.7(2) . . . . ?
C3 Tc1 C5 C4 150.3(2) 3 . . . ?
C1 Tc1 C5 C4 -103.5(3) . . . . ?
C1 Tc1 C5 C4 76.5(3) 3 . . . ?
C5 Tc1 C5 C6 -107(5) 3 . . . ?
C4 Tc1 C5 C6 132.5(4) . . . . ?
C4 Tc1 C5 C6 -47.5(4) 3 . . . ?
C2 Tc1 C5 C6 66.1(2) . . . . ?
C2 Tc1 C5 C6 -113.9(2) 3 . . . ?
C6 Tc1 C5 C6 180.0 3 . . . ?
C3 Tc1 C5 C6 102.8(3) . . . . ?
C3 Tc1 C5 C6 -77.2(3) 3 . . . ?
C1 Tc1 C5 C6 29.0(2) . . . . ?
C1 Tc1 C5 C6 -151.0(2) 3 . . . ?
C4 C5 C6 C1 -0.3(6) . . . . ?
Tc1 C5 C6 C1 -54.9(3) . . . . ?
C4 C5 C6 Tc1 54.6(4) . . . . ?
C2 C1 C6 C5 -0.3(5) . . . . ?
C7 C1 C6 C5 180.0(4) . . . . ?
Tc1 C1 C6 C5 54.5(3) . . . . ?
C2 C1 C6 Tc1 -54.8(3) . . . . ?
C7 C1 C6 Tc1 125.5(4) . . . . ?
C5 Tc1 C6 C5 179.998(1) 3 . . . ?
C4 Tc1 C6 C5 -28.7(2) . . . . ?
C4 Tc1 C6 C5 151.3(2) 3 . . . ?
C2 Tc1 C6 C5 -102.1(3) . . . . ?
C2 Tc1 C6 C5 77.9(3) 3 . . . ?
C6 Tc1 C6 C5 -107(2) 3 . . . ?
C3 Tc1 C6 C5 -65.4(2) . . . . ?
C3 Tc1 C6 C5 114.6(2) 3 . . . ?
C1 Tc1 C6 C5 -132.4(3) . . . . ?
C1 Tc1 C6 C5 47.6(3) 3 . . . ?
C5 Tc1 C6 C1 -47.6(3) 3 . . . ?
C5 Tc1 C6 C1 132.4(3) . . . . ?
C4 Tc1 C6 C1 103.8(2) . . . . ?
C4 Tc1 C6 C1 -76.2(2) 3 . . . ?
C2 Tc1 C6 C1 30.4(2) . . . . ?
C2 Tc1 C6 C1 -149.6(2) 3 . . . ?
C6 Tc1 C6 C1 25(2) 3 . . . ?
C3 Tc1 C6 C1 67.0(2) . . . . ?
C3 Tc1 C6 C1 -113.0(2) 3 . . . ?
C1 Tc1 C6 C1 180.0 3 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 1017766'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_c:[tc(mesitylene)2](pf6)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Tc(mesitylene)2]PF6'
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H24 Tc F6 P'
_chemical_formula_sum            'C18 H24 F6 P Tc'
_chemical_formula_weight         483.34

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'
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'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   9.2697(5)
_cell_length_b                   13.0695(16)
_cell_length_c                   15.815(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1916.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    5887
_cell_measurement_theta_min      2.7870
_cell_measurement_theta_max      32.6170

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6877
_exptl_absorpt_correction_T_max  0.9077
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
; 
 none 
;

_diffrn_ambient_temperature      183(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  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12954
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         30.51
_reflns_number_total             5851
_reflns_number_gt                5484
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0225P)²+0.0000P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_number_reflns         5851
_refine_ls_number_parameters     277
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0642
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.006
_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
Tc1 Tc 0.552636(19) 0.991582(13) 0.907021(11) 0.01730(5) Uani 1 1 d . . .
C1 C 0.7847(3) 1.03938(19) 0.91846(18) 0.0286(6) Uani 1 1 d . . .
C2 C 0.6951(3) 1.1110(2) 0.96136(17) 0.0300(6) Uani 1 1 d . . .
H2A H 0.7133 1.1253 1.0193 0.036 Uiso 1 1 calc R . .
C3 C 0.5803(3) 1.16131(18) 0.92056(18) 0.0298(6) Uani 1 1 d . . .
C4 C 0.5533(4) 1.13750(17) 0.83507(17) 0.0305(6) Uani 1 1 d . . .
H4A H 0.4746 1.1692 0.8069 0.037 Uiso 1 1 calc R . .
C5 C 0.6410(3) 1.0675(2) 0.79061(17) 0.0306(6) Uani 1 1 d . . .
C6 C 0.7546(3) 1.0190(2) 0.83308(15) 0.0275(6) Uani 1 1 d . . .
H6A H 0.8127 0.9711 0.8034 0.033 Uiso 1 1 calc R . .
C7 C 0.9089(3) 0.9884(3) 0.96184(18) 0.0409(7) Uani 1 1 d . . .
H7A H 0.8898 0.9846 1.0227 0.049 Uiso 1 1 calc R . .
H7B H 0.9971 1.0281 0.9520 0.049 Uiso 1 1 calc R . .
H7C H 0.9213 0.9192 0.9392 0.049 Uiso 1 1 calc R . .
C8 C 0.4881(4) 1.2383(2) 0.9643(2) 0.0469(9) Uani 1 1 d . . .
H8A H 0.3896 1.2346 0.9419 0.056 Uiso 1 1 calc R . .
H8B H 0.5271 1.3070 0.9545 0.056 Uiso 1 1 calc R . .
H8C H 0.4868 1.2240 1.0251 0.056 Uiso 1 1 calc R . .
C9 C 0.6135(4) 1.0466(3) 0.69832(17) 0.0481(9) Uani 1 1 d . . .
H9A H 0.6421 0.9762 0.6849 0.058 Uiso 1 1 calc R . .
H9B H 0.6699 1.0944 0.6638 0.058 Uiso 1 1 calc R . .
H9C H 0.5106 1.0556 0.6861 0.058 Uiso 1 1 calc R . .
C11 C 0.5525(3) 0.83419(18) 0.96467(18) 0.0297(6) Uani 1 1 d . . .
C12 C 0.4838(3) 0.9035(2) 1.02051(16) 0.0288(6) Uani 1 1 d . . .
H12A H 0.5176 0.9094 1.0770 0.035 Uiso 1 1 calc R . .
C13 C 0.3662(3) 0.96399(19) 0.99392(17) 0.0279(6) Uani 1 1 d . . .
C14 C 0.3191(2) 0.95589(18) 0.90892(18) 0.0257(5) Uani 1 1 d . . .
H14A H 0.2418 0.9975 0.8897 0.031 Uiso 1 1 calc R . .
C15 C 0.3854(3) 0.88694(19) 0.85255(17) 0.0264(6) Uani 1 1 d . . .
C16 C 0.5035(3) 0.82789(18) 0.88057(18) 0.0266(6) Uani 1 1 d . . .
H16A H 0.5506 0.7832 0.8421 0.032 Uiso 1 1 calc R . .
C17 C 0.6754(3) 0.7683(2) 0.9949(3) 0.0512(9) Uani 1 1 d . . .
H17A H 0.7428 0.7565 0.9482 0.061 Uiso 1 1 calc R . .
H17B H 0.6376 0.7026 1.0149 0.061 Uiso 1 1 calc R . .
H17C H 0.7257 0.8029 1.0413 0.061 Uiso 1 1 calc R . .
C18 C 0.2929(3) 1.0348(3) 1.05441(19) 0.0459(8) Uani 1 1 d . . .
H18A H 0.3634 1.0610 1.0952 0.055 Uiso 1 1 calc R . .
H18B H 0.2166 0.9978 1.0845 0.055 Uiso 1 1 calc R . .
H18C H 0.2504 1.0921 1.0232 0.055 Uiso 1 1 calc R . .
C19 C 0.3300(4) 0.8772(2) 0.76332(18) 0.0452(8) Uani 1 1 d . . .
H19C H 0.2567 0.8232 0.7609 0.054 Uiso 1 1 calc R . .
H19B H 0.4100 0.8597 0.7255 0.054 Uiso 1 1 calc R . .
H19A H 0.2872 0.9423 0.7455 0.054 Uiso 1 1 calc R . .
P1 P 0.10713(10) 1.22074(6) 0.76654(6) 0.0397(2) Uani 1 1 d . . .
F1 F 0.1413(3) 1.16263(17) 0.85174(14) 0.0771(7) Uani 1 1 d . A .
F4 F 0.0788(3) 1.28075(17) 0.68173(14) 0.0833(9) Uani 1 1 d . A .
F2B F 0.1728(19) 1.3182(11) 0.8005(12) 0.147(8) Uani 0.40 1 d P A 1
F3B F -0.0415(13) 1.2464(8) 0.8142(8) 0.085(3) Uani 0.40 1 d P A 1
F5B F 0.0309(18) 1.1159(11) 0.7383(11) 0.102(5) Uani 0.40 1 d P A 1
F6B F 0.2420(16) 1.1801(13) 0.7224(12) 0.128(8) Uani 0.40 1 d P A 1
F2A F 0.2473(8) 1.2916(7) 0.7876(8) 0.077(2) Uani 0.60 1 d P A 2
F3A F 0.0121(8) 1.3016(6) 0.8104(5) 0.092(3) Uani 0.60 1 d P A 2
F5A F -0.0201(10) 1.1530(7) 0.7394(8) 0.093(3) Uani 0.60 1 d P A 2
F6A F 0.2186(12) 1.1467(7) 0.7205(7) 0.088(3) Uani 0.60 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 C14 2.214(2) . ?
Tc1 C2 2.218(3) . ?
Tc1 C4 2.221(2) . ?
Tc1 C12 2.226(2) . ?
Tc1 C16 2.227(2) . ?
Tc1 C6 2.236(2) . ?
Tc1 C13 2.237(2) . ?
Tc1 C15 2.239(3) . ?
Tc1 C3 2.243(2) . ?
Tc1 C5 2.246(3) . ?
Tc1 C1 2.248(2) . ?
Tc1 C11 2.250(2) . ?
C1 C6 1.405(3) . ?
C1 C2 1.424(4) . ?
C1 C7 1.496(3) . ?
C2 C3 1.407(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.410(4) . ?
C3 C8 1.491(4) . ?
C4 C5 1.412(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.401(4) . ?
C5 C9 1.507(4) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C16 1.408(4) . ?
C11 C12 1.417(4) . ?
C11 C17 1.506(4) . ?
C12 C13 1.410(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.417(4) . ?
C13 C18 1.495(4) . ?
C14 C15 1.409(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.410(4) . ?
C15 C19 1.507(4) . ?
C16 H16A 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19C 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19A 0.9800 . ?
P1 F2B 1.511(14) . ?
P1 F6B 1.528(11) . ?
P1 F5A 1.536(10) . ?
P1 F3A 1.541(7) . ?
P1 F4 1.576(2) . ?
P1 F1 1.579(2) . ?
P1 F6A 1.592(8) . ?
P1 F3B 1.606(12) . ?
P1 F5B 1.606(15) . ?
P1 F2A 1.630(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
C14 Tc1 C2 136.47(10) . . ?
C14 Tc1 C4 100.98(11) . . ?
C2 Tc1 C4 65.96(11) . . ?
C14 Tc1 C12 66.42(10) . . ?
C2 Tc1 C12 102.84(10) . . ?
C4 Tc1 C12 149.11(11) . . ?
C14 Tc1 C16 66.43(10) . . ?
C2 Tc1 C16 150.55(10) . . ?
C4 Tc1 C16 136.82(10) . . ?
C12 Tc1 C16 66.17(10) . . ?
C14 Tc1 C6 149.22(10) . . ?
C2 Tc1 C6 65.89(10) . . ?
C4 Tc1 C6 65.95(10) . . ?
C12 Tc1 C6 138.11(10) . . ?
C16 Tc1 C6 103.11(10) . . ?
C14 Tc1 C13 37.13(10) . . ?
C2 Tc1 C13 109.59(10) . . ?
C4 Tc1 C13 117.08(11) . . ?
C12 Tc1 C13 36.85(9) . . ?
C16 Tc1 C13 78.60(10) . . ?
C6 Tc1 C13 173.57(10) . . ?
C14 Tc1 C15 36.87(9) . . ?
C2 Tc1 C15 172.30(10) . . ?
C4 Tc1 C15 109.22(11) . . ?
C12 Tc1 C15 78.23(10) . . ?
C16 Tc1 C15 36.81(9) . . ?
C6 Tc1 C15 118.42(10) . . ?
C13 Tc1 C15 66.63(10) . . ?
C14 Tc1 C3 108.60(10) . . ?
C2 Tc1 C3 36.77(10) . . ?
C4 Tc1 C3 36.82(9) . . ?
C12 Tc1 C3 117.86(10) . . ?
C16 Tc1 C3 172.42(11) . . ?
C6 Tc1 C3 78.22(10) . . ?
C13 Tc1 C3 100.91(10) . . ?
C15 Tc1 C3 136.04(10) . . ?
C14 Tc1 C5 117.43(10) . . ?
C2 Tc1 C5 77.86(10) . . ?
C4 Tc1 C5 36.85(10) . . ?
C12 Tc1 C5 173.73(11) . . ?
C16 Tc1 C5 110.18(10) . . ?
C6 Tc1 C5 36.43(9) . . ?
C13 Tc1 C5 148.92(11) . . ?
C15 Tc1 C5 101.93(10) . . ?
C3 Tc1 C5 66.41(10) . . ?
C14 Tc1 C1 173.27(10) . . ?
C2 Tc1 C1 37.18(10) . . ?
C4 Tc1 C1 78.47(11) . . ?
C12 Tc1 C1 110.68(10) . . ?
C16 Tc1 C1 118.56(10) . . ?
C6 Tc1 C1 36.51(9) . . ?
C13 Tc1 C1 137.28(10) . . ?
C15 Tc1 C1 149.68(10) . . ?
C3 Tc1 C1 66.92(10) . . ?
C5 Tc1 C1 66.06(11) . . ?
C14 Tc1 C11 78.55(10) . . ?
C2 Tc1 C11 119.12(11) . . ?
C4 Tc1 C11 173.08(10) . . ?
C12 Tc1 C11 36.90(10) . . ?
C16 Tc1 C11 36.66(10) . . ?
C6 Tc1 C11 111.01(10) . . ?
C13 Tc1 C11 66.63(10) . . ?
C15 Tc1 C11 66.25(10) . . ?
C3 Tc1 C11 149.93(11) . . ?
C5 Tc1 C11 137.40(10) . . ?
C1 Tc1 C11 102.82(10) . . ?
C6 C1 C2 117.8(2) . . ?
C6 C1 C7 120.6(3) . . ?
C2 C1 C7 121.6(3) . . ?
C6 C1 Tc1 71.31(14) . . ?
C2 C1 Tc1 70.27(14) . . ?
C7 C1 Tc1 130.51(18) . . ?
C3 C2 C1 122.0(2) . . ?
C3 C2 Tc1 72.59(15) . . ?
C1 C2 Tc1 72.55(14) . . ?
C3 C2 H2A 119.0 . . ?
C1 C2 H2A 119.0 . . ?
Tc1 C2 H2A 128.2 . . ?
C2 C3 C4 118.1(2) . . ?
C2 C3 C8 122.4(3) . . ?
C4 C3 C8 119.4(3) . . ?
C2 C3 Tc1 70.64(14) . . ?
C4 C3 Tc1 70.72(13) . . ?
C8 C3 Tc1 130.3(2) . . ?
C3 C4 C5 121.2(3) . . ?
C3 C4 Tc1 72.46(14) . . ?
C5 C4 Tc1 72.55(14) . . ?
C3 C4 H4A 119.4 . . ?
C5 C4 H4A 119.4 . . ?
Tc1 C4 H4A 127.8 . . ?
C6 C5 C4 119.2(3) . . ?
C6 C5 C9 120.6(3) . . ?
C4 C5 C9 120.2(3) . . ?
C6 C5 Tc1 71.42(14) . . ?
C4 C5 Tc1 70.61(14) . . ?
C9 C5 Tc1 130.7(2) . . ?
C5 C6 C1 121.6(2) . . ?
C5 C6 Tc1 72.15(15) . . ?
C1 C6 Tc1 72.19(14) . . ?
C5 C6 H6A 119.2 . . ?
C1 C6 H6A 119.2 . . ?
Tc1 C6 H6A 128.9 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C16 C11 C12 118.8(3) . . ?
C16 C11 C17 120.7(3) . . ?
C12 C11 C17 120.5(3) . . ?
C16 C11 Tc1 70.79(14) . . ?
C12 C11 Tc1 70.62(14) . . ?
C17 C11 Tc1 130.6(2) . . ?
C13 C12 C11 121.3(2) . . ?
C13 C12 Tc1 72.01(14) . . ?
C11 C12 Tc1 72.48(14) . . ?
C13 C12 H12A 119.3 . . ?
C11 C12 H12A 119.3 . . ?
Tc1 C12 H12A 128.5 . . ?
C12 C13 C14 118.6(2) . . ?
C12 C13 C18 120.5(3) . . ?
C14 C13 C18 120.9(3) . . ?
C12 C13 Tc1 71.14(14) . . ?
C14 C13 Tc1 70.56(14) . . ?
C18 C13 Tc1 130.15(19) . . ?
C15 C14 C13 120.9(2) . . ?
C15 C14 Tc1 72.53(14) . . ?
C13 C14 Tc1 72.31(14) . . ?
C15 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
Tc1 C14 H14A 127.8 . . ?
C14 C15 C16 119.3(2) . . ?
C14 C15 C19 119.9(3) . . ?
C16 C15 C19 120.8(3) . . ?
C14 C15 Tc1 70.59(14) . . ?
C16 C15 Tc1 71.12(15) . . ?
C19 C15 Tc1 130.39(19) . . ?
C11 C16 C15 121.0(2) . . ?
C11 C16 Tc1 72.56(14) . . ?
C15 C16 Tc1 72.07(13) . . ?
C11 C16 H16A 119.5 . . ?
C15 C16 H16A 119.5 . . ?
Tc1 C16 H16A 128.1 . . ?
C11 C17 H17A 109.5 . . ?
C11 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C11 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19C 109.5 . . ?
C15 C19 H19B 109.5 . . ?
H19C C19 H19B 109.5 . . ?
C15 C19 H19A 109.5 . . ?
H19C C19 H19A 109.5 . . ?
H19B C19 H19A 109.5 . . ?
F2B P1 F6B 97.2(10) . . ?
F2B P1 F5A 153.5(8) . . ?
F6B P1 F5A 107.5(8) . . ?
F2B P1 F3A 59.5(7) . . ?
F6B P1 F3A 155.8(7) . . ?
F5A P1 F3A 94.7(5) . . ?
F2B P1 F4 87.1(6) . . ?
F6B P1 F4 85.5(7) . . ?
F5A P1 F4 85.5(5) . . ?
F3A P1 F4 87.0(3) . . ?
F2B P1 F1 91.2(6) . . ?
F6B P1 F1 93.4(7) . . ?
F5A P1 F1 96.6(5) . . ?
F3A P1 F1 93.4(3) . . ?
F4 P1 F1 177.83(16) . . ?
F2B P1 F6A 114.4(8) . . ?
F6B P1 F6A 17.8(9) . . ?
F5A P1 F6A 91.2(5) . . ?
F3A P1 F6A 173.7(5) . . ?
F4 P1 F6A 91.2(5) . . ?
F1 P1 F6A 88.2(5) . . ?
F2B P1 F3B 90.2(8) . . ?
F6B P1 F3B 171.7(8) . . ?
F5A P1 F3B 66.0(6) . . ?
F3A P1 F3B 32.3(4) . . ?
F4 P1 F3B 98.8(4) . . ?
F1 P1 F3B 82.7(4) . . ?
F6A P1 F3B 154.0(5) . . ?
F2B P1 F5B 175.0(10) . . ?
F6B P1 F5B 86.3(8) . . ?
F5A P1 F5B 24.8(7) . . ?
F3A P1 F5B 117.3(6) . . ?
F4 P1 F5B 96.6(6) . . ?
F1 P1 F5B 85.1(6) . . ?
F6A P1 F5B 68.9(7) . . ?
F3B P1 F5B 86.1(7) . . ?
F2B P1 F2A 29.2(8) . . ?
F6B P1 F2A 68.8(8) . . ?
F5A P1 F2A 175.4(6) . . ?
F3A P1 F2A 88.5(5) . . ?
F4 P1 F2A 91.4(4) . . ?
F1 P1 F2A 86.5(4) . . ?
F6A P1 F2A 85.5(5) . . ?
F3B P1 F2A 118.0(5) . . ?
F5B P1 F2A 153.2(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 Tc1 C1 C6 -150.9(7) . . . . ?
C2 Tc1 C1 C6 -130.2(2) . . . . ?
C4 Tc1 C1 C6 -64.95(16) . . . . ?
C12 Tc1 C1 C6 145.83(15) . . . . ?
C16 Tc1 C1 C6 72.47(17) . . . . ?
C13 Tc1 C1 C6 177.41(15) . . . . ?
C15 Tc1 C1 C6 43.5(3) . . . . ?
C3 Tc1 C1 C6 -101.71(17) . . . . ?
C5 Tc1 C1 C6 -28.37(15) . . . . ?
C11 Tc1 C1 C6 108.09(16) . . . . ?
C14 Tc1 C1 C2 -20.7(9) . . . . ?
C4 Tc1 C1 C2 65.22(16) . . . . ?
C12 Tc1 C1 C2 -83.99(17) . . . . ?
C16 Tc1 C1 C2 -157.36(16) . . . . ?
C6 Tc1 C1 C2 130.2(2) . . . . ?
C13 Tc1 C1 C2 -52.4(2) . . . . ?
C15 Tc1 C1 C2 173.68(18) . . . . ?
C3 Tc1 C1 C2 28.47(15) . . . . ?
C5 Tc1 C1 C2 101.80(18) . . . . ?
C11 Tc1 C1 C2 -121.74(17) . . . . ?
C14 Tc1 C1 C7 94.4(8) . . . . ?
C2 Tc1 C1 C7 115.1(3) . . . . ?
C4 Tc1 C1 C7 -179.6(3) . . . . ?
C12 Tc1 C1 C7 31.1(3) . . . . ?
C16 Tc1 C1 C7 -42.2(3) . . . . ?
C6 Tc1 C1 C7 -114.7(3) . . . . ?
C13 Tc1 C1 C7 62.7(3) . . . . ?
C15 Tc1 C1 C7 -71.2(3) . . . . ?
C3 Tc1 C1 C7 143.6(3) . . . . ?
C5 Tc1 C1 C7 -143.1(3) . . . . ?
C11 Tc1 C1 C7 -6.6(3) . . . . ?
C6 C1 C2 C3 -0.6(4) . . . . ?
C7 C1 C2 C3 178.4(2) . . . . ?
Tc1 C1 C2 C3 -55.5(2) . . . . ?
C6 C1 C2 Tc1 54.9(2) . . . . ?
C7 C1 C2 Tc1 -126.1(2) . . . . ?
C14 Tc1 C2 C3 -50.6(2) . . . . ?
C4 Tc1 C2 C3 29.84(16) . . . . ?
C12 Tc1 C2 C3 -119.71(17) . . . . ?
C16 Tc1 C2 C3 176.34(18) . . . . ?
C6 Tc1 C2 C3 103.03(17) . . . . ?
C13 Tc1 C2 C3 -81.90(18) . . . . ?
C15 Tc1 C2 C3 -22.6(8) . . . . ?
C5 Tc1 C2 C3 66.68(17) . . . . ?
C1 Tc1 C2 C3 132.9(2) . . . . ?
C11 Tc1 C2 C3 -155.42(17) . . . . ?
C14 Tc1 C2 C1 176.54(16) . . . . ?
C4 Tc1 C2 C1 -103.06(18) . . . . ?
C12 Tc1 C2 C1 107.39(16) . . . . ?
C16 Tc1 C2 C1 43.4(3) . . . . ?
C6 Tc1 C2 C1 -29.87(15) . . . . ?
C13 Tc1 C2 C1 145.20(15) . . . . ?
C15 Tc1 C2 C1 -155.5(7) . . . . ?
C3 Tc1 C2 C1 -132.9(2) . . . . ?
C5 Tc1 C2 C1 -66.22(17) . . . . ?
C11 Tc1 C2 C1 71.68(19) . . . . ?
C1 C2 C3 C4 1.3(4) . . . . ?
Tc1 C2 C3 C4 -54.2(2) . . . . ?
C1 C2 C3 C8 -178.5(3) . . . . ?
Tc1 C2 C3 C8 126.0(3) . . . . ?
C1 C2 C3 Tc1 55.5(2) . . . . ?
C14 Tc1 C3 C2 145.86(16) . . . . ?
C4 Tc1 C3 C2 -130.7(3) . . . . ?
C12 Tc1 C3 C2 73.30(18) . . . . ?
C16 Tc1 C3 C2 -166.2(7) . . . . ?
C6 Tc1 C3 C2 -65.28(16) . . . . ?
C13 Tc1 C3 C2 108.22(17) . . . . ?
C15 Tc1 C3 C2 175.75(16) . . . . ?
C5 Tc1 C3 C2 -101.59(18) . . . . ?
C1 Tc1 C3 C2 -28.76(16) . . . . ?
C11 Tc1 C3 C2 46.5(3) . . . . ?
C14 Tc1 C3 C4 -83.45(19) . . . . ?
C2 Tc1 C3 C4 130.7(3) . . . . ?
C12 Tc1 C3 C4 -156.01(18) . . . . ?
C16 Tc1 C3 C4 -35.5(8) . . . . ?
C6 Tc1 C3 C4 65.41(18) . . . . ?
C13 Tc1 C3 C4 -121.09(18) . . . . ?
C15 Tc1 C3 C4 -53.6(2) . . . . ?
C5 Tc1 C3 C4 29.10(18) . . . . ?
C1 Tc1 C3 C4 101.93(19) . . . . ?
C11 Tc1 C3 C4 177.2(2) . . . . ?
C14 Tc1 C3 C8 29.3(3) . . . . ?
C2 Tc1 C3 C8 -116.6(3) . . . . ?
C4 Tc1 C3 C8 112.7(4) . . . . ?
C12 Tc1 C3 C8 -43.3(3) . . . . ?
C16 Tc1 C3 C8 77.2(8) . . . . ?
C6 Tc1 C3 C8 178.1(3) . . . . ?
C13 Tc1 C3 C8 -8.4(3) . . . . ?
C15 Tc1 C3 C8 59.2(3) . . . . ?
C5 Tc1 C3 C8 141.8(3) . . . . ?
C1 Tc1 C3 C8 -145.4(3) . . . . ?
C11 Tc1 C3 C8 -70.1(4) . . . . ?
C2 C3 C4 C5 -1.8(4) . . . . ?
C8 C3 C4 C5 177.9(3) . . . . ?
Tc1 C3 C4 C5 -56.0(2) . . . . ?
C2 C3 C4 Tc1 54.2(2) . . . . ?
C8 C3 C4 Tc1 -126.1(2) . . . . ?
C14 Tc1 C4 C3 106.43(18) . . . . ?
C2 Tc1 C4 C3 -29.80(16) . . . . ?
C12 Tc1 C4 C3 44.4(3) . . . . ?
C16 Tc1 C4 C3 173.57(16) . . . . ?
C6 Tc1 C4 C3 -102.90(19) . . . . ?
C13 Tc1 C4 C3 70.8(2) . . . . ?
C15 Tc1 C4 C3 143.75(17) . . . . ?
C5 Tc1 C4 C3 -132.0(3) . . . . ?
C1 Tc1 C4 C3 -66.73(18) . . . . ?
C11 Tc1 C4 C3 -168.1(9) . . . . ?
C14 Tc1 C4 C5 -121.57(18) . . . . ?
C2 Tc1 C4 C5 102.20(19) . . . . ?
C12 Tc1 C4 C5 176.43(19) . . . . ?
C16 Tc1 C4 C5 -54.4(2) . . . . ?
C6 Tc1 C4 C5 29.10(16) . . . . ?
C13 Tc1 C4 C5 -157.18(17) . . . . ?
C15 Tc1 C4 C5 -84.26(19) . . . . ?
C3 Tc1 C4 C5 132.0(3) . . . . ?
C1 Tc1 C4 C5 65.27(18) . . . . ?
C11 Tc1 C4 C5 -36.1(11) . . . . ?
C3 C4 C5 C6 1.7(4) . . . . ?
Tc1 C4 C5 C6 -54.3(2) . . . . ?
C3 C4 C5 C9 -177.5(2) . . . . ?
Tc1 C4 C5 C9 126.5(3) . . . . ?
C3 C4 C5 Tc1 56.0(2) . . . . ?
C14 Tc1 C5 C6 -157.96(15) . . . . ?
C2 Tc1 C5 C6 65.66(17) . . . . ?
C4 Tc1 C5 C6 131.6(3) . . . . ?
C12 Tc1 C5 C6 -31.4(10) . . . . ?
C16 Tc1 C5 C6 -84.78(17) . . . . ?
C13 Tc1 C5 C6 173.57(17) . . . . ?
C15 Tc1 C5 C6 -122.21(16) . . . . ?
C3 Tc1 C5 C6 102.51(17) . . . . ?
C1 Tc1 C5 C6 28.43(15) . . . . ?
C11 Tc1 C5 C6 -54.4(2) . . . . ?
C14 Tc1 C5 C4 70.45(19) . . . . ?
C2 Tc1 C5 C4 -65.93(18) . . . . ?
C12 Tc1 C5 C4 -163.0(9) . . . . ?
C16 Tc1 C5 C4 143.63(17) . . . . ?
C6 Tc1 C5 C4 -131.6(3) . . . . ?
C13 Tc1 C5 C4 42.0(3) . . . . ?
C15 Tc1 C5 C4 106.20(18) . . . . ?
C3 Tc1 C5 C4 -29.08(17) . . . . ?
C1 Tc1 C5 C4 -103.16(19) . . . . ?
C11 Tc1 C5 C4 173.97(19) . . . . ?
C14 Tc1 C5 C9 -43.1(3) . . . . ?
C2 Tc1 C5 C9 -179.5(3) . . . . ?
C4 Tc1 C5 C9 -113.6(4) . . . . ?
C12 Tc1 C5 C9 83.4(10) . . . . ?
C16 Tc1 C5 C9 30.1(3) . . . . ?
C6 Tc1 C5 C9 114.8(3) . . . . ?
C13 Tc1 C5 C9 -71.6(3) . . . . ?
C15 Tc1 C5 C9 -7.4(3) . . . . ?
C3 Tc1 C5 C9 -142.6(3) . . . . ?
C1 Tc1 C5 C9 143.3(3) . . . . ?
C11 Tc1 C5 C9 60.4(3) . . . . ?
C4 C5 C6 C1 -0.9(4) . . . . ?
C9 C5 C6 C1 178.2(2) . . . . ?
Tc1 C5 C6 C1 -54.9(2) . . . . ?
C4 C5 C6 Tc1 53.9(2) . . . . ?
C9 C5 C6 Tc1 -126.9(2) . . . . ?
C2 C1 C6 C5 0.4(4) . . . . ?
C7 C1 C6 C5 -178.5(2) . . . . ?
Tc1 C1 C6 C5 54.8(2) . . . . ?
C2 C1 C6 Tc1 -54.4(2) . . . . ?
C7 C1 C6 Tc1 126.6(2) . . . . ?
C14 Tc1 C6 C5 40.6(3) . . . . ?
C2 Tc1 C6 C5 -102.61(18) . . . . ?
C4 Tc1 C6 C5 -29.42(16) . . . . ?
C12 Tc1 C6 C5 175.11(16) . . . . ?
C16 Tc1 C6 C5 106.31(16) . . . . ?
C13 Tc1 C6 C5 -148.9(8) . . . . ?
C15 Tc1 C6 C5 70.27(18) . . . . ?
C3 Tc1 C6 C5 -66.05(17) . . . . ?
C1 Tc1 C6 C5 -133.0(2) . . . . ?
C11 Tc1 C6 C5 143.85(16) . . . . ?
C14 Tc1 C6 C1 173.61(15) . . . . ?
C2 Tc1 C6 C1 30.39(15) . . . . ?
C4 Tc1 C6 C1 103.59(17) . . . . ?
C12 Tc1 C6 C1 -51.9(2) . . . . ?
C16 Tc1 C6 C1 -120.69(16) . . . . ?
C13 Tc1 C6 C1 -15.9(9) . . . . ?
C15 Tc1 C6 C1 -156.72(15) . . . . ?
C3 Tc1 C6 C1 66.95(16) . . . . ?
C5 Tc1 C6 C1 133.0(2) . . . . ?
C11 Tc1 C6 C1 -83.15(17) . . . . ?
C14 Tc1 C11 C16 65.72(17) . . . . ?
C2 Tc1 C11 C16 -157.06(16) . . . . ?
C4 Tc1 C11 C16 -21.1(11) . . . . ?
C12 Tc1 C11 C16 131.5(3) . . . . ?
C6 Tc1 C11 C16 -83.74(18) . . . . ?
C13 Tc1 C11 C16 102.72(18) . . . . ?
C15 Tc1 C11 C16 29.10(16) . . . . ?
C3 Tc1 C11 C16 173.15(19) . . . . ?
C5 Tc1 C11 C16 -52.6(2) . . . . ?
C1 Tc1 C11 C16 -121.03(17) . . . . ?
C14 Tc1 C11 C12 -65.79(17) . . . . ?
C2 Tc1 C11 C12 71.4(2) . . . . ?
C4 Tc1 C11 C12 -152.6(10) . . . . ?
C16 Tc1 C11 C12 -131.5(3) . . . . ?
C6 Tc1 C11 C12 144.76(16) . . . . ?
C13 Tc1 C11 C12 -28.79(16) . . . . ?
C15 Tc1 C11 C12 -102.41(18) . . . . ?
C3 Tc1 C11 C12 41.6(3) . . . . ?
C5 Tc1 C11 C12 175.92(16) . . . . ?
C1 Tc1 C11 C12 107.47(17) . . . . ?
C14 Tc1 C11 C17 -179.9(3) . . . . ?
C2 Tc1 C11 C17 -42.6(3) . . . . ?
C4 Tc1 C11 C17 93.4(11) . . . . ?
C12 Tc1 C11 C17 -114.1(4) . . . . ?
C16 Tc1 C11 C17 114.4(4) . . . . ?
C6 Tc1 C11 C17 30.7(3) . . . . ?
C13 Tc1 C11 C17 -142.9(3) . . . . ?
C15 Tc1 C11 C17 143.5(3) . . . . ?
C3 Tc1 C11 C17 -72.4(4) . . . . ?
C5 Tc1 C11 C17 61.9(3) . . . . ?
C1 Tc1 C11 C17 -6.6(3) . . . . ?
C16 C11 C12 C13 1.4(4) . . . . ?
C17 C11 C12 C13 -178.4(3) . . . . ?
Tc1 C11 C12 C13 55.2(2) . . . . ?
C16 C11 C12 Tc1 -53.8(2) . . . . ?
C17 C11 C12 Tc1 126.5(3) . . . . ?
C14 Tc1 C12 C13 -29.76(15) . . . . ?
C2 Tc1 C12 C13 105.63(16) . . . . ?
C4 Tc1 C12 C13 41.3(3) . . . . ?
C16 Tc1 C12 C13 -103.25(17) . . . . ?
C6 Tc1 C12 C13 173.70(15) . . . . ?
C15 Tc1 C12 C13 -66.57(16) . . . . ?
C3 Tc1 C12 C13 69.61(18) . . . . ?
C5 Tc1 C12 C13 -158.7(9) . . . . ?
C1 Tc1 C12 C13 143.68(15) . . . . ?
C11 Tc1 C12 C13 -132.5(2) . . . . ?
C14 Tc1 C12 C11 102.75(18) . . . . ?
C2 Tc1 C12 C11 -121.86(18) . . . . ?
C4 Tc1 C12 C11 173.8(2) . . . . ?
C16 Tc1 C12 C11 29.26(17) . . . . ?
C6 Tc1 C12 C11 -53.8(2) . . . . ?
C13 Tc1 C12 C11 132.5(2) . . . . ?
C15 Tc1 C12 C11 65.94(17) . . . . ?
C3 Tc1 C12 C11 -157.88(16) . . . . ?
C5 Tc1 C12 C11 -26.2(10) . . . . ?
C1 Tc1 C12 C11 -83.81(18) . . . . ?
C11 C12 C13 C14 -1.3(4) . . . . ?
Tc1 C12 C13 C14 54.1(2) . . . . ?
C11 C12 C13 C18 178.5(3) . . . . ?
Tc1 C12 C13 C18 -126.1(2) . . . . ?
C11 C12 C13 Tc1 -55.4(2) . . . . ?
C14 Tc1 C13 C12 131.1(2) . . . . ?
C2 Tc1 C13 C12 -85.32(17) . . . . ?
C4 Tc1 C13 C12 -157.64(16) . . . . ?
C16 Tc1 C13 C12 65.27(16) . . . . ?
C6 Tc1 C13 C12 -40.9(9) . . . . ?
C15 Tc1 C13 C12 101.89(17) . . . . ?
C3 Tc1 C13 C12 -122.44(16) . . . . ?
C5 Tc1 C13 C12 175.59(19) . . . . ?
C1 Tc1 C13 C12 -54.8(2) . . . . ?
C11 Tc1 C13 C12 28.82(15) . . . . ?
C2 Tc1 C13 C14 143.59(15) . . . . ?
C4 Tc1 C13 C14 71.28(17) . . . . ?
C12 Tc1 C13 C14 -131.1(2) . . . . ?
C16 Tc1 C13 C14 -65.82(15) . . . . ?
C6 Tc1 C13 C14 -171.9(8) . . . . ?
C15 Tc1 C13 C14 -29.20(15) . . . . ?
C3 Tc1 C13 C14 106.47(16) . . . . ?
C5 Tc1 C13 C14 44.5(3) . . . . ?
C1 Tc1 C13 C14 174.15(13) . . . . ?
C11 Tc1 C13 C14 -102.26(17) . . . . ?
C14 Tc1 C13 C18 -114.5(3) . . . . ?
C2 Tc1 C13 C18 29.1(3) . . . . ?
C4 Tc1 C13 C18 -43.2(3) . . . . ?
C12 Tc1 C13 C18 114.5(3) . . . . ?
C16 Tc1 C13 C18 179.7(3) . . . . ?
C6 Tc1 C13 C18 73.6(9) . . . . ?
C15 Tc1 C13 C18 -143.7(3) . . . . ?
C3 Tc1 C13 C18 -8.0(3) . . . . ?
C5 Tc1 C13 C18 -70.0(3) . . . . ?
C1 Tc1 C13 C18 59.7(3) . . . . ?
C11 Tc1 C13 C18 143.3(3) . . . . ?
C12 C13 C14 C15 1.7(4) . . . . ?
C18 C13 C14 C15 -178.1(2) . . . . ?
Tc1 C13 C14 C15 56.1(2) . . . . ?
C12 C13 C14 Tc1 -54.3(2) . . . . ?
C18 C13 C14 Tc1 125.8(2) . . . . ?
C2 Tc1 C14 C15 173.99(15) . . . . ?
C4 Tc1 C14 C15 107.46(17) . . . . ?
C12 Tc1 C14 C15 -102.18(17) . . . . ?
C16 Tc1 C14 C15 -29.07(15) . . . . ?
C6 Tc1 C14 C15 46.5(2) . . . . ?
C13 Tc1 C14 C15 -131.7(2) . . . . ?
C3 Tc1 C14 C15 144.80(15) . . . . ?
C5 Tc1 C14 C15 72.32(17) . . . . ?
C1 Tc1 C14 C15 -167.9(7) . . . . ?
C11 Tc1 C14 C15 -65.50(16) . . . . ?
C2 Tc1 C14 C13 -54.3(2) . . . . ?
C4 Tc1 C14 C13 -120.80(15) . . . . ?
C12 Tc1 C14 C13 29.55(14) . . . . ?
C16 Tc1 C14 C13 102.66(16) . . . . ?
C6 Tc1 C14 C13 178.24(17) . . . . ?
C15 Tc1 C14 C13 131.7(2) . . . . ?
C3 Tc1 C14 C13 -83.47(16) . . . . ?
C5 Tc1 C14 C13 -155.95(15) . . . . ?
C1 Tc1 C14 C13 -36.2(8) . . . . ?
C11 Tc1 C14 C13 66.24(15) . . . . ?
C13 C14 C15 C16 -2.2(4) . . . . ?
Tc1 C14 C15 C16 53.8(2) . . . . ?
C13 C14 C15 C19 177.9(2) . . . . ?
Tc1 C14 C15 C19 -126.2(2) . . . . ?
C13 C14 C15 Tc1 -56.0(2) . . . . ?
C2 Tc1 C15 C14 -32.6(8) . . . . ?
C4 Tc1 C15 C14 -82.62(17) . . . . ?
C12 Tc1 C15 C14 66.22(16) . . . . ?
C16 Tc1 C15 C14 132.0(2) . . . . ?
C6 Tc1 C15 C14 -155.03(15) . . . . ?
C13 Tc1 C15 C14 29.39(15) . . . . ?
C3 Tc1 C15 C14 -51.9(2) . . . . ?
C5 Tc1 C15 C14 -120.19(16) . . . . ?
C1 Tc1 C15 C14 177.21(18) . . . . ?
C11 Tc1 C15 C14 103.01(17) . . . . ?
C14 Tc1 C15 C16 -132.0(2) . . . . ?
C2 Tc1 C15 C16 -164.6(7) . . . . ?
C4 Tc1 C15 C16 145.40(17) . . . . ?
C12 Tc1 C15 C16 -65.77(17) . . . . ?
C6 Tc1 C15 C16 72.98(18) . . . . ?
C13 Tc1 C15 C16 -102.60(17) . . . . ?
C3 Tc1 C15 C16 176.09(15) . . . . ?
C5 Tc1 C15 C16 107.82(17) . . . . ?
C1 Tc1 C15 C16 45.2(3) . . . . ?
C11 Tc1 C15 C16 -28.98(16) . . . . ?
C14 Tc1 C15 C19 113.2(3) . . . . ?
C2 Tc1 C15 C19 80.6(8) . . . . ?
C4 Tc1 C15 C19 30.6(3) . . . . ?
C12 Tc1 C15 C19 179.4(3) . . . . ?
C16 Tc1 C15 C19 -114.8(3) . . . . ?
C6 Tc1 C15 C19 -41.9(3) . . . . ?
C13 Tc1 C15 C19 142.6(3) . . . . ?
C3 Tc1 C15 C19 61.3(3) . . . . ?
C5 Tc1 C15 C19 -7.0(3) . . . . ?
C1 Tc1 C15 C19 -69.6(4) . . . . ?
C11 Tc1 C15 C19 -143.8(3) . . . . ?
C12 C11 C16 C15 -1.9(4) . . . . ?
C17 C11 C16 C15 177.9(2) . . . . ?
Tc1 C11 C16 C15 -55.6(2) . . . . ?
C12 C11 C16 Tc1 53.7(2) . . . . ?
C17 C11 C16 Tc1 -126.5(3) . . . . ?
C14 C15 C16 C11 2.3(4) . . . . ?
C19 C15 C16 C11 -177.8(3) . . . . ?
Tc1 C15 C16 C11 55.8(2) . . . . ?
C14 C15 C16 Tc1 -53.5(2) . . . . ?
C19 C15 C16 Tc1 126.4(2) . . . . ?
C14 Tc1 C16 C11 -102.91(18) . . . . ?
C2 Tc1 C16 C11 43.8(3) . . . . ?
C4 Tc1 C16 C11 176.37(19) . . . . ?
C12 Tc1 C16 C11 -29.44(17) . . . . ?
C6 Tc1 C16 C11 107.67(17) . . . . ?
C13 Tc1 C16 C11 -65.99(17) . . . . ?
C15 Tc1 C16 C11 -132.0(2) . . . . ?
C3 Tc1 C16 C11 -153.0(7) . . . . ?
C5 Tc1 C16 C11 145.06(17) . . . . ?
C1 Tc1 C16 C11 72.05(19) . . . . ?
C14 Tc1 C16 C15 29.12(16) . . . . ?
C2 Tc1 C16 C15 175.85(18) . . . . ?
C4 Tc1 C16 C15 -51.6(2) . . . . ?
C12 Tc1 C16 C15 102.59(18) . . . . ?
C6 Tc1 C16 C15 -120.30(16) . . . . ?
C13 Tc1 C16 C15 66.04(16) . . . . ?
C3 Tc1 C16 C15 -21.0(8) . . . . ?
C5 Tc1 C16 C15 -82.91(17) . . . . ?
C1 Tc1 C16 C15 -155.92(16) . . . . ?
C11 Tc1 C16 C15 132.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 1017767'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_c:\[tc(tetralin)2](pf6)

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Tc(teralin)2]PF6'
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H24 Tc, F6 P'
_chemical_formula_sum            'C20 H24 F6 P Tc'
_chemical_formula_weight         507.36

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'
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'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   8.7563(6)
_cell_length_b                   12.1899(11)
_cell_length_c                   9.5187(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.089(10)
_cell_angle_gamma                90.00
_cell_volume                     965.80(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    3129
_cell_measurement_theta_min      3.1760
_cell_measurement_theta_max      32.4520

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             512
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6318
_exptl_absorpt_correction_T_max  0.8495
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 none
;

_diffrn_ambient_temperature      183(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  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6611
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         30.51
_reflns_number_total             2906
_reflns_number_gt                2360
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0553P)²+0.4935P] where P=(Fo²+2Fc²)/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         2906
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1065
_refine_ls_wR_factor_gt          0.0986
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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
Tc1 Tc 0.5000 0.0000 0.5000 0.02423(10) Uani 1 2 d S . .
C1 C 0.4966(3) -0.0692(2) 0.7146(3) 0.0418(6) Uani 1 1 d . . .
H1A H 0.5821 -0.0727 0.8050 0.050 Uiso 1 1 calc R . .
C2 C 0.4744(4) -0.1554(2) 0.6139(4) 0.0485(7) Uani 1 1 d . . .
H2A H 0.5439 -0.2172 0.6366 0.058 Uiso 1 1 calc R . .
C3 C 0.3511(4) -0.1511(2) 0.4806(4) 0.0472(7) Uani 1 1 d . . .
H3A H 0.3362 -0.2099 0.4121 0.057 Uiso 1 1 calc R . .
C4 C 0.2479(3) -0.0593(2) 0.4471(3) 0.0370(5) Uani 1 1 d . . .
H4A H 0.1642 -0.0564 0.3554 0.044 Uiso 1 1 calc R . .
C5 C 0.2679(3) 0.0288(2) 0.5490(3) 0.0293(4) Uani 1 1 d . . .
C6 C 0.3930(3) 0.0244(2) 0.6843(3) 0.0317(4) Uani 1 1 d . . .
C7 C 0.4164(3) 0.1170(3) 0.7935(3) 0.0509(7) Uani 1 1 d . . .
H7A H 0.5326 0.1326 0.8362 0.061 Uiso 1 1 calc R . .
H7B H 0.3752 0.0947 0.8750 0.061 Uiso 1 1 calc R . .
C8 C 0.3277(4) 0.2230(3) 0.7194(4) 0.0615(9) Uani 1 1 d . . .
H8A H 0.3286 0.2773 0.7970 0.074 Uiso 1 1 calc R . .
H8B H 0.3857 0.2553 0.6552 0.074 Uiso 1 1 calc R . .
C9 C 0.1592(4) 0.2001(3) 0.6300(4) 0.0554(7) Uani 1 1 d . . .
H9A H 0.1044 0.2698 0.5907 0.066 Uiso 1 1 calc R . .
H9B H 0.1014 0.1661 0.6933 0.066 Uiso 1 1 calc R . .
C10 C 0.1540(3) 0.1252(2) 0.5053(3) 0.0431(6) Uani 1 1 d . . .
H10B H 0.1806 0.1675 0.4272 0.052 Uiso 1 1 calc R . .
H10A H 0.0431 0.0970 0.4627 0.052 Uiso 1 1 calc R . .
P1 P 0.5000 0.5000 0.5000 0.0310(2) Uani 1 2 d S . .
F1 F 0.3743(3) 0.40721(15) 0.4175(3) 0.0631(6) Uani 1 1 d . A .
F2A F 0.3896(15) 0.5932(9) 0.3932(11) 0.069(2) Uani 0.60 1 d P A 1
F2B F 0.368(2) 0.5867(13) 0.4378(17) 0.071(4) Uani 0.40 1 d P A 2
F3A F 0.4323(12) 0.4946(10) 0.6368(13) 0.085(3) Uani 0.60 1 d P A 1
F3B F 0.405(2) 0.5199(16) 0.610(2) 0.102(7) Uani 0.40 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 C1 2.219(2) . ?
Tc1 C1 2.219(2) 3_656 ?
Tc1 C4 2.227(2) . ?
Tc1 C4 2.227(2) 3_656 ?
Tc1 C2 2.228(2) 3_656 ?
Tc1 C2 2.228(2) . ?
Tc1 C3 2.231(2) 3_656 ?
Tc1 C3 2.231(2) . ?
Tc1 C5 2.250(2) . ?
Tc1 C5 2.250(2) 3_656 ?
Tc1 C6 2.250(2) 3_656 ?
Tc1 C6 2.250(2) . ?
C1 C2 1.394(4) . ?
C1 C6 1.430(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.389(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.411(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.422(3) . ?
C4 H4A 0.9500 . ?
C5 C6 1.409(3) . ?
C5 C10 1.513(3) . ?
C6 C7 1.505(4) . ?
C7 C8 1.559(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.483(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.487(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10B 0.9900 . ?
C10 H10A 0.9900 . ?
P1 F3B 1.539(13) 3_666 ?
P1 F3B 1.539(13) . ?
P1 F2B 1.542(14) . ?
P1 F2B 1.542(14) 3_666 ?
P1 F3A 1.590(11) . ?
P1 F3A 1.590(11) 3_666 ?
P1 F1 1.6034(18) . ?
P1 F1 1.6035(18) 3_666 ?
P1 F2A 1.628(10) . ?
P1 F2A 1.628(10) 3_666 ?
F2B F3B 1.76(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Tc1 C1 180.0 . 3_656 ?
C1 Tc1 C4 77.82(10) . . ?
C1 Tc1 C4 102.18(10) 3_656 . ?
C1 Tc1 C4 102.18(10) . 3_656 ?
C1 Tc1 C4 77.82(10) 3_656 3_656 ?
C4 Tc1 C4 180.0 . 3_656 ?
C1 Tc1 C2 143.46(11) . 3_656 ?
C1 Tc1 C2 36.54(11) 3_656 3_656 ?
C4 Tc1 C2 114.10(11) . 3_656 ?
C4 Tc1 C2 65.89(11) 3_656 3_656 ?
C1 Tc1 C2 36.54(11) . . ?
C1 Tc1 C2 143.46(11) 3_656 . ?
C4 Tc1 C2 65.90(11) . . ?
C4 Tc1 C2 114.10(11) 3_656 . ?
C2 Tc1 C2 180.00(7) 3_656 . ?
C1 Tc1 C3 114.34(11) . 3_656 ?
C1 Tc1 C3 65.65(11) 3_656 3_656 ?
C4 Tc1 C3 143.10(10) . 3_656 ?
C4 Tc1 C3 36.90(10) 3_656 3_656 ?
C2 Tc1 C3 36.29(12) 3_656 3_656 ?
C2 Tc1 C3 143.71(12) . 3_656 ?
C1 Tc1 C3 65.65(11) . . ?
C1 Tc1 C3 114.35(11) 3_656 . ?
C4 Tc1 C3 36.90(10) . . ?
C4 Tc1 C3 143.10(10) 3_656 . ?
C2 Tc1 C3 143.71(12) 3_656 . ?
C2 Tc1 C3 36.29(12) . . ?
C3 Tc1 C3 180.0 3_656 . ?
C1 Tc1 C5 66.25(9) . . ?
C1 Tc1 C5 113.75(9) 3_656 . ?
C4 Tc1 C5 37.03(9) . . ?
C4 Tc1 C5 142.97(9) 3_656 . ?
C2 Tc1 C5 101.66(9) 3_656 . ?
C2 Tc1 C5 78.34(9) . . ?
C3 Tc1 C5 113.35(9) 3_656 . ?
C3 Tc1 C5 66.65(9) . . ?
C1 Tc1 C5 113.75(9) . 3_656 ?
C1 Tc1 C5 66.25(9) 3_656 3_656 ?
C4 Tc1 C5 142.97(9) . 3_656 ?
C4 Tc1 C5 37.03(9) 3_656 3_656 ?
C2 Tc1 C5 78.34(9) 3_656 3_656 ?
C2 Tc1 C5 101.66(9) . 3_656 ?
C3 Tc1 C5 66.65(9) 3_656 3_656 ?
C3 Tc1 C5 113.35(9) . 3_656 ?
C5 Tc1 C5 180.00(11) . 3_656 ?
C1 Tc1 C6 142.69(9) . 3_656 ?
C1 Tc1 C6 37.31(9) 3_656 3_656 ?
C4 Tc1 C6 113.84(9) . 3_656 ?
C4 Tc1 C6 66.16(9) 3_656 3_656 ?
C2 Tc1 C6 66.66(10) 3_656 3_656 ?
C2 Tc1 C6 113.34(10) . 3_656 ?
C3 Tc1 C6 78.43(9) 3_656 3_656 ?
C3 Tc1 C6 101.57(9) . 3_656 ?
C5 Tc1 C6 143.50(9) . 3_656 ?
C5 Tc1 C6 36.50(9) 3_656 3_656 ?
C1 Tc1 C6 37.31(9) . . ?
C1 Tc1 C6 142.69(9) 3_656 . ?
C4 Tc1 C6 66.16(9) . . ?
C4 Tc1 C6 113.84(9) 3_656 . ?
C2 Tc1 C6 113.35(10) 3_656 . ?
C2 Tc1 C6 66.65(10) . . ?
C3 Tc1 C6 101.57(9) 3_656 . ?
C3 Tc1 C6 78.43(9) . . ?
C5 Tc1 C6 36.50(9) . . ?
C5 Tc1 C6 143.50(9) 3_656 . ?
C6 Tc1 C6 180.0 3_656 . ?
C2 C1 C6 121.2(2) . . ?
C2 C1 Tc1 72.10(15) . . ?
C6 C1 Tc1 72.52(13) . . ?
C2 C1 H1A 119.4 . . ?
C6 C1 H1A 119.4 . . ?
Tc1 C1 H1A 128.2 . . ?
C3 C2 C1 120.2(2) . . ?
C3 C2 Tc1 71.96(14) . . ?
C1 C2 Tc1 71.36(13) . . ?
C3 C2 H2A 119.9 . . ?
C1 C2 H2A 119.9 . . ?
Tc1 C2 H2A 129.1 . . ?
C2 C3 C4 119.9(2) . . ?
C2 C3 Tc1 71.75(14) . . ?
C4 C3 Tc1 71.39(13) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
Tc1 C3 H3A 129.1 . . ?
C3 C4 C5 120.7(2) . . ?
C3 C4 Tc1 71.71(14) . . ?
C5 C4 Tc1 72.36(12) . . ?
C3 C4 H4A 119.6 . . ?
C5 C4 H4A 119.6 . . ?
Tc1 C4 H4A 128.6 . . ?
C6 C5 C4 119.4(2) . . ?
C6 C5 C10 122.7(2) . . ?
C4 C5 C10 117.9(2) . . ?
C6 C5 Tc1 71.77(13) . . ?
C4 C5 Tc1 70.61(12) . . ?
C10 C5 Tc1 128.68(17) . . ?
C5 C6 C1 118.7(2) . . ?
C5 C6 C7 120.2(2) . . ?
C1 C6 C7 121.1(2) . . ?
C5 C6 Tc1 71.74(13) . . ?
C1 C6 Tc1 70.16(14) . . ?
C7 C6 Tc1 129.57(17) . . ?
C6 C7 C8 111.6(2) . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C9 C8 C7 111.8(2) . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
C8 C9 C10 110.6(2) . . ?
C8 C9 H9A 109.5 . . ?
C10 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C9 C10 C5 113.8(2) . . ?
C9 C10 H10B 108.8 . . ?
C5 C10 H10B 108.8 . . ?
C9 C10 H10A 108.8 . . ?
C5 C10 H10A 108.8 . . ?
H10B C10 H10A 107.7 . . ?
F3B P1 F3B 179.999(5) 3_666 . ?
F3B P1 F2B 110.1(10) 3_666 . ?
F3B P1 F2B 69.9(10) . . ?
F3B P1 F2B 69.9(10) 3_666 3_666 ?
F3B P1 F2B 110.1(10) . 3_666 ?
F2B P1 F2B 179.999(4) . 3_666 ?
F3B P1 F3A 164.6(12) 3_666 . ?
F3B P1 F3A 15.4(12) . . ?
F2B P1 F3A 85.3(7) . . ?
F2B P1 F3A 94.7(7) 3_666 . ?
F3B P1 F3A 15.4(12) 3_666 3_666 ?
F3B P1 F3A 164.6(12) . 3_666 ?
F2B P1 F3A 94.7(7) . 3_666 ?
F2B P1 F3A 85.3(7) 3_666 3_666 ?
F3A P1 F3A 180.0(6) . 3_666 ?
F3B P1 F1 89.4(7) 3_666 . ?
F3B P1 F1 90.6(7) . . ?
F2B P1 F1 88.7(7) . . ?
F2B P1 F1 91.3(7) 3_666 . ?
F3A P1 F1 89.9(3) . . ?
F3A P1 F1 90.1(3) 3_666 . ?
F3B P1 F1 90.6(7) 3_666 3_666 ?
F3B P1 F1 89.4(7) . 3_666 ?
F2B P1 F1 91.3(7) . 3_666 ?
F2B P1 F1 88.7(7) 3_666 3_666 ?
F3A P1 F1 90.1(3) . 3_666 ?
F3A P1 F1 89.9(3) 3_666 3_666 ?
F1 P1 F1 180.0 . 3_666 ?
F3B P1 F2A 91.5(9) 3_666 . ?
F3B P1 F2A 88.5(9) . . ?
F2B P1 F2A 18.7(8) . . ?
F2B P1 F2A 161.3(8) 3_666 . ?
F3A P1 F2A 103.9(6) . . ?
F3A P1 F2A 76.1(6) 3_666 . ?
F1 P1 F2A 90.1(4) . . ?
F1 P1 F2A 89.9(4) 3_666 . ?
F3B P1 F2A 88.5(9) 3_666 3_666 ?
F3B P1 F2A 91.5(9) . 3_666 ?
F2B P1 F2A 161.3(8) . 3_666 ?
F2B P1 F2A 18.7(8) 3_666 3_666 ?
F3A P1 F2A 76.1(6) . 3_666 ?
F3A P1 F2A 103.9(6) 3_666 3_666 ?
F1 P1 F2A 89.9(4) . 3_666 ?
F1 P1 F2A 90.1(4) 3_666 3_666 ?
F2A P1 F2A 179.999(2) . 3_666 ?
P1 F2B F3B 55.0(6) . . ?
P1 F3B F2B 55.1(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Tc1 C1 C2 154(15) 3_656 . . . ?
C4 Tc1 C1 C2 65.77(16) . . . . ?
C4 Tc1 C1 C2 -114.23(16) 3_656 . . . ?
C2 Tc1 C1 C2 180.0 3_656 . . . ?
C3 Tc1 C1 C2 -151.07(16) 3_656 . . . ?
C3 Tc1 C1 C2 28.93(16) . . . . ?
C5 Tc1 C1 C2 102.89(17) . . . . ?
C5 Tc1 C1 C2 -77.11(17) 3_656 . . . ?
C6 Tc1 C1 C2 -47.7(2) 3_656 . . . ?
C6 Tc1 C1 C2 132.3(2) . . . . ?
C1 Tc1 C1 C6 22(15) 3_656 . . . ?
C4 Tc1 C1 C6 -66.49(16) . . . . ?
C4 Tc1 C1 C6 113.51(16) 3_656 . . . ?
C2 Tc1 C1 C6 47.7(2) 3_656 . . . ?
C2 Tc1 C1 C6 -132.3(2) . . . . ?
C3 Tc1 C1 C6 76.67(17) 3_656 . . . ?
C3 Tc1 C1 C6 -103.33(17) . . . . ?
C5 Tc1 C1 C6 -29.37(14) . . . . ?
C5 Tc1 C1 C6 150.63(14) 3_656 . . . ?
C6 Tc1 C1 C6 180.002(1) 3_656 . . . ?
C6 C1 C2 C3 0.7(4) . . . . ?
Tc1 C1 C2 C3 -55.0(2) . . . . ?
C6 C1 C2 Tc1 55.6(2) . . . . ?
C1 Tc1 C2 C3 131.9(2) . . . . ?
C1 Tc1 C2 C3 -48.1(2) 3_656 . . . ?
C4 Tc1 C2 C3 29.44(14) . . . . ?
C4 Tc1 C2 C3 -150.56(14) 3_656 . . . ?
C2 Tc1 C2 C3 -140(13) 3_656 . . . ?
C3 Tc1 C2 C3 180.0 3_656 . . . ?
C5 Tc1 C2 C3 66.24(15) . . . . ?
C5 Tc1 C2 C3 -113.76(15) 3_656 . . . ?
C6 Tc1 C2 C3 -77.36(16) 3_656 . . . ?
C6 Tc1 C2 C3 102.63(16) . . . . ?
C1 Tc1 C2 C1 180.0 3_656 . . . ?
C4 Tc1 C2 C1 -102.44(16) . . . . ?
C4 Tc1 C2 C1 77.56(16) 3_656 . . . ?
C2 Tc1 C2 C1 88(13) 3_656 . . . ?
C3 Tc1 C2 C1 48.1(2) 3_656 . . . ?
C3 Tc1 C2 C1 -131.9(2) . . . . ?
C5 Tc1 C2 C1 -65.65(15) . . . . ?
C5 Tc1 C2 C1 114.35(15) 3_656 . . . ?
C6 Tc1 C2 C1 150.75(15) 3_656 . . . ?
C6 Tc1 C2 C1 -29.25(15) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
Tc1 C2 C3 C4 -54.8(2) . . . . ?
C1 C2 C3 Tc1 54.7(2) . . . . ?
C1 Tc1 C3 C2 -29.11(15) . . . . ?
C1 Tc1 C3 C2 150.89(15) 3_656 . . . ?
C4 Tc1 C3 C2 -131.6(2) . . . . ?
C4 Tc1 C3 C2 48.4(2) 3_656 . . . ?
C2 Tc1 C3 C2 180.0 3_656 . . . ?
C3 Tc1 C3 C2 -17(21) 3_656 . . . ?
C5 Tc1 C3 C2 -102.48(16) . . . . ?
C5 Tc1 C3 C2 77.52(16) 3_656 . . . ?
C6 Tc1 C3 C2 113.87(16) 3_656 . . . ?
C6 Tc1 C3 C2 -66.13(16) . . . . ?
C1 Tc1 C3 C4 102.53(16) . . . . ?
C1 Tc1 C3 C4 -77.47(16) 3_656 . . . ?
C4 Tc1 C3 C4 180.0 3_656 . . . ?
C2 Tc1 C3 C4 -48.4(2) 3_656 . . . ?
C2 Tc1 C3 C4 131.6(2) . . . . ?
C3 Tc1 C3 C4 115(21) 3_656 . . . ?
C5 Tc1 C3 C4 29.16(14) . . . . ?
C5 Tc1 C3 C4 -150.84(14) 3_656 . . . ?
C6 Tc1 C3 C4 -114.49(15) 3_656 . . . ?
C6 Tc1 C3 C4 65.51(15) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
Tc1 C3 C4 C5 -55.42(19) . . . . ?
C2 C3 C4 Tc1 54.9(2) . . . . ?
C1 Tc1 C4 C3 -65.49(17) . . . . ?
C1 Tc1 C4 C3 114.51(17) 3_656 . . . ?
C4 Tc1 C4 C3 132(7) 3_656 . . . ?
C2 Tc1 C4 C3 151.01(16) 3_656 . . . ?
C2 Tc1 C4 C3 -28.99(16) . . . . ?
C3 Tc1 C4 C3 180.0 3_656 . . . ?
C5 Tc1 C4 C3 -132.0(2) . . . . ?
C5 Tc1 C4 C3 48.0(2) 3_656 . . . ?
C6 Tc1 C4 C3 77.09(17) 3_656 . . . ?
C6 Tc1 C4 C3 -102.91(17) . . . . ?
C1 Tc1 C4 C5 66.54(16) . . . . ?
C1 Tc1 C4 C5 -113.46(16) 3_656 . . . ?
C4 Tc1 C4 C5 -96(7) 3_656 . . . ?
C2 Tc1 C4 C5 -76.96(17) 3_656 . . . ?
C2 Tc1 C4 C5 103.04(17) . . . . ?
C3 Tc1 C4 C5 -48.0(2) 3_656 . . . ?
C3 Tc1 C4 C5 132.0(2) . . . . ?
C5 Tc1 C4 C5 180.0 3_656 . . . ?
C6 Tc1 C4 C5 -150.89(14) 3_656 . . . ?
C6 Tc1 C4 C5 29.11(14) . . . . ?
C3 C4 C5 C6 0.5(3) . . . . ?
Tc1 C4 C5 C6 -54.64(19) . . . . ?
C3 C4 C5 C10 179.4(2) . . . . ?
Tc1 C4 C5 C10 124.3(2) . . . . ?
C3 C4 C5 Tc1 55.12(19) . . . . ?
C1 Tc1 C5 C6 29.99(15) . . . . ?
C1 Tc1 C5 C6 -150.01(15) 3_656 . . . ?
C4 Tc1 C5 C6 131.6(2) . . . . ?
C4 Tc1 C5 C6 -48.4(2) 3_656 . . . ?
C2 Tc1 C5 C6 -113.67(16) 3_656 . . . ?
C2 Tc1 C5 C6 66.33(16) . . . . ?
C3 Tc1 C5 C6 -77.50(17) 3_656 . . . ?
C3 Tc1 C5 C6 102.50(17) . . . . ?
C5 Tc1 C5 C6 -99.4(14) 3_656 . . . ?
C6 Tc1 C5 C6 180.0 3_656 . . . ?
C1 Tc1 C5 C4 -101.57(17) . . . . ?
C1 Tc1 C5 C4 78.43(17) 3_656 . . . ?
C4 Tc1 C5 C4 180.0 3_656 . . . ?
C2 Tc1 C5 C4 114.77(17) 3_656 . . . ?
C2 Tc1 C5 C4 -65.23(17) . . . . ?
C3 Tc1 C5 C4 150.93(16) 3_656 . . . ?
C3 Tc1 C5 C4 -29.07(16) . . . . ?
C5 Tc1 C5 C4 129.1(18) 3_656 . . . ?
C6 Tc1 C5 C4 48.4(2) 3_656 . . . ?
C6 Tc1 C5 C4 -131.6(2) . . . . ?
C1 Tc1 C5 C10 147.7(2) . . . . ?
C1 Tc1 C5 C10 -32.3(2) 3_656 . . . ?
C4 Tc1 C5 C10 -110.7(3) . . . . ?
C4 Tc1 C5 C10 69.3(3) 3_656 . . . ?
C2 Tc1 C5 C10 4.0(2) 3_656 . . . ?
C2 Tc1 C5 C10 -176.0(2) . . . . ?
C3 Tc1 C5 C10 40.2(3) 3_656 . . . ?
C3 Tc1 C5 C10 -139.8(3) . . . . ?
C5 Tc1 C5 C10 18.3(19) 3_656 . . . ?
C6 Tc1 C5 C10 -62.3(3) 3_656 . . . ?
C6 Tc1 C5 C10 117.7(3) . . . . ?
C4 C5 C6 C1 0.1(3) . . . . ?
C10 C5 C6 C1 -178.8(2) . . . . ?
Tc1 C5 C6 C1 -54.00(19) . . . . ?
C4 C5 C6 C7 179.8(2) . . . . ?
C10 C5 C6 C7 1.0(3) . . . . ?
Tc1 C5 C6 C7 125.7(2) . . . . ?
C4 C5 C6 Tc1 54.09(18) . . . . ?
C10 C5 C6 Tc1 -124.8(2) . . . . ?
C2 C1 C6 C5 -0.7(3) . . . . ?
Tc1 C1 C6 C5 54.76(19) . . . . ?
C2 C1 C6 C7 179.6(2) . . . . ?
Tc1 C1 C6 C7 -125.0(2) . . . . ?
C2 C1 C6 Tc1 -55.4(2) . . . . ?
C1 Tc1 C6 C5 -131.0(2) . . . . ?
C1 Tc1 C6 C5 49.0(2) 3_656 . . . ?
C4 Tc1 C6 C5 -29.51(14) . . . . ?
C4 Tc1 C6 C5 150.49(14) 3_656 . . . ?
C2 Tc1 C6 C5 77.68(17) 3_656 . . . ?
C2 Tc1 C6 C5 -102.32(17) . . . . ?
C3 Tc1 C6 C5 113.81(16) 3_656 . . . ?
C3 Tc1 C6 C5 -66.19(16) . . . . ?
C5 Tc1 C6 C5 180.0 3_656 . . . ?
C6 Tc1 C6 C5 -56(5) 3_656 . . . ?
C1 Tc1 C6 C1 180.000(1) 3_656 . . . ?
C4 Tc1 C6 C1 101.49(18) . . . . ?
C4 Tc1 C6 C1 -78.51(18) 3_656 . . . ?
C2 Tc1 C6 C1 -151.32(17) 3_656 . . . ?
C2 Tc1 C6 C1 28.68(17) . . . . ?
C3 Tc1 C6 C1 -115.19(17) 3_656 . . . ?
C3 Tc1 C6 C1 64.81(17) . . . . ?
C5 Tc1 C6 C1 131.0(2) . . . . ?
C5 Tc1 C6 C1 -49.0(2) 3_656 . . . ?
C6 Tc1 C6 C1 75(5) 3_656 . . . ?
C1 Tc1 C6 C7 114.5(3) . . . . ?
C1 Tc1 C6 C7 -65.5(3) 3_656 . . . ?
C4 Tc1 C6 C7 -144.0(3) . . . . ?
C4 Tc1 C6 C7 36.0(3) 3_656 . . . ?
C2 Tc1 C6 C7 -36.8(3) 3_656 . . . ?
C2 Tc1 C6 C7 143.2(3) . . . . ?
C3 Tc1 C6 C7 -0.7(3) 3_656 . . . ?
C3 Tc1 C6 C7 179.3(3) . . . . ?
C5 Tc1 C6 C7 -114.5(3) . . . . ?
C5 Tc1 C6 C7 65.5(3) 3_656 . . . ?
C6 Tc1 C6 C7 -170(5) 3_656 . . . ?
C5 C6 C7 C8 -17.4(3) . . . . ?
C1 C6 C7 C8 162.3(2) . . . . ?
Tc1 C6 C7 C8 73.2(3) . . . . ?
C6 C7 C8 C9 48.5(3) . . . . ?
C7 C8 C9 C10 -63.2(3) . . . . ?
C8 C9 C10 C5 44.9(3) . . . . ?
C6 C5 C10 C9 -14.4(3) . . . . ?
C4 C5 C10 C9 166.7(2) . . . . ?
Tc1 C5 C10 C9 -106.6(3) . . . . ?
F3B P1 F2B F3B 179.999(10) 3_666 . . . ?
F2B P1 F2B F3B 80(12) 3_666 . . . ?
F3A P1 F2B F3B 1.1(11) . . . . ?
F3A P1 F2B F3B -178.9(11) 3_666 . . . ?
F1 P1 F2B F3B 91.2(8) . . . . ?
F1 P1 F2B F3B -88.8(8) 3_666 . . . ?
F2A P1 F2B F3B -175(4) . . . . ?
F2A P1 F2B F3B 5(4) 3_666 . . . ?
F3B P1 F3B F2B -146(12) 3_666 . . . ?
F2B P1 F3B F2B 180.001(7) 3_666 . . . ?
F3A P1 F3B F2B -176(4) . . . . ?
F3A P1 F3B F2B 4(4) 3_666 . . . ?
F1 P1 F3B F2B -88.4(8) . . . . ?
F1 P1 F3B F2B 91.6(8) 3_666 . . . ?
F2A P1 F3B F2B 1.7(12) . . . . ?
F2A P1 F3B F2B -178.3(12) 3_666 . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.532
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.117
_database_code_depnum_ccdc_archive 'CCDC 1017768'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_meb310114

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H49 Al Cl7 N7 O7 Tc'
_chemical_formula_weight         884.80

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21

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

_cell_length_a                   8.8724(3)
_cell_length_b                   23.5963(7)
_cell_length_c                   9.6318(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.888(3)
_cell_angle_gamma                90.00
_cell_volume                     2001.92(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    9721
_cell_measurement_theta_min      2.8950
_cell_measurement_theta_max      31.8090

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             910
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5148
_exptl_absorpt_correction_T_max  0.8793
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(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  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18867
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         26.37
_reflns_number_total             8169
_reflns_number_gt                7662
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0284P)²+0.0000P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_number_reflns         8169
_refine_ls_number_parameters     411
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0674
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
Tc1 Tc -0.04364(2) -0.110519(9) -0.50601(2) 0.01970(6) Uani 1 1 d . . .
Cl1 Cl 0.01424(9) -0.01309(3) -0.51655(9) 0.03244(18) Uani 1 1 d . . .
Cl2 Cl -0.20488(8) -0.09041(3) -0.33471(8) 0.02923(17) Uani 1 1 d . . .
Cl3 Cl -0.10957(10) -0.20692(3) -0.49683(9) 0.03422(19) Uani 1 1 d . . .
Cl4 Cl 0.12313(8) -0.13158(3) -0.67158(8) 0.03038(17) Uani 1 1 d . . .
Cl5 Cl -0.24250(8) -0.09634(3) -0.68810(9) 0.0354(2) Uani 1 1 d . . .
Cl6 Cl 0.15467(8) -0.12554(3) -0.32473(8) 0.03088(19) Uani 1 1 d . . .
Al1 Al 0.28807(11) 0.14565(3) 0.24962(9) 0.02027(19) Uani 1 1 d . . .
O1 O 0.3890(2) 0.20696(8) 0.3426(2) 0.0233(4) Uani 1 1 d . . .
O2 O 0.1119(2) 0.15678(8) 0.3388(2) 0.0276(5) Uani 1 1 d . . .
O3 O 0.1848(2) 0.08399(8) 0.1581(2) 0.0256(5) Uani 1 1 d . . .
O4 O 0.4564(3) 0.13293(8) 0.1503(2) 0.0264(5) Uani 1 1 d . . .
O5 O 0.2078(2) 0.19498(8) 0.1069(2) 0.0240(4) Uani 1 1 d . . .
O6 O 0.3803(2) 0.09784(8) 0.3884(2) 0.0262(5) Uani 1 1 d . . .
C1 C 0.4218(3) 0.21470(12) 0.4726(3) 0.0224(6) Uani 1 1 d . . .
H1 H 0.3960 0.1861 0.5351 0.027 Uiso 1 1 calc R . .
C2 C 0.5270(4) 0.30633(13) 0.4334(4) 0.0386(8) Uani 1 1 d . . .
H2A H 0.4488 0.3358 0.4304 0.046 Uiso 1 1 calc R . .
H2B H 0.5317 0.2916 0.3388 0.046 Uiso 1 1 calc R . .
H2C H 0.6256 0.3225 0.4696 0.046 Uiso 1 1 calc R . .
C3 C 0.5128(4) 0.27060(15) 0.6736(4) 0.0392(8) Uani 1 1 d . . .
H3C H 0.6212 0.2762 0.7036 0.047 Uiso 1 1 calc R . .
H3B H 0.4763 0.2379 0.7229 0.047 Uiso 1 1 calc R . .
H3A H 0.4566 0.3046 0.6955 0.047 Uiso 1 1 calc R . .
C4 C 0.0824(4) 0.14845(13) 0.4616(3) 0.0311(7) Uani 1 1 d . . .
H4 H 0.1593 0.1331 0.5282 0.037 Uiso 1 1 calc R . .
C5 C -0.1695(4) 0.1859(2) 0.4090(5) 0.0679(13) Uani 1 1 d . . .
H5A H -0.1467 0.1832 0.3122 0.081 Uiso 1 1 calc R . .
H5B H -0.1785 0.2259 0.4343 0.081 Uiso 1 1 calc R . .
H5C H -0.2653 0.1664 0.4181 0.081 Uiso 1 1 calc R . .
C6 C -0.0727(6) 0.1523(2) 0.6453(5) 0.0782(17) Uani 1 1 d . . .
H6C H -0.1063 0.1881 0.6831 0.094 Uiso 1 1 calc R . .
H6B H 0.0226 0.1403 0.6993 0.094 Uiso 1 1 calc R . .
H6A H -0.1504 0.1232 0.6517 0.094 Uiso 1 1 calc R . .
C7 C 0.1755(3) 0.06964(12) 0.0326(3) 0.0268(7) Uani 1 1 d . . .
H7 H 0.2291 0.0909 -0.0294 0.032 Uiso 1 1 calc R . .
C8 C 0.0079(4) -0.00769(14) 0.0737(4) 0.0397(9) Uani 1 1 d . . .
H8A H -0.0048 0.0137 0.1587 0.048 Uiso 1 1 calc R . .
H8B H 0.0626 -0.0430 0.0990 0.048 Uiso 1 1 calc R . .
H8C H -0.0921 -0.0166 0.0237 0.048 Uiso 1 1 calc R . .
C9 C 0.0856(5) 0.01020(18) -0.1629(4) 0.0615(13) Uani 1 1 d . . .
H9C H -0.0191 0.0144 -0.2073 0.074 Uiso 1 1 calc R . .
H9B H 0.1175 -0.0293 -0.1701 0.074 Uiso 1 1 calc R . .
H9A H 0.1526 0.0347 -0.2101 0.074 Uiso 1 1 calc R . .
C10 C 0.5308(3) 0.16921(13) 0.0917(3) 0.0292(7) Uani 1 1 d . . .
H10 H 0.4919 0.2067 0.0816 0.035 Uiso 1 1 calc R . .
C11 C 0.7175(6) 0.10091(19) 0.0494(7) 0.089(2) Uani 1 1 d . . .
H11A H 0.7128 0.0858 -0.0458 0.107 Uiso 1 1 calc R . .
H11B H 0.6567 0.0770 0.1046 0.107 Uiso 1 1 calc R . .
H11C H 0.8232 0.1012 0.0928 0.107 Uiso 1 1 calc R . .
C12 C 0.7382(5) 0.20026(19) -0.0278(5) 0.0640(13) Uani 1 1 d . . .
H12C H 0.8456 0.2005 0.0104 0.077 Uiso 1 1 calc R . .
H12B H 0.6940 0.2377 -0.0147 0.077 Uiso 1 1 calc R . .
H12A H 0.7289 0.1913 -0.1278 0.077 Uiso 1 1 calc R . .
C13 C 0.1544(3) 0.24459(12) 0.1177(3) 0.0245(6) Uani 1 1 d . . .
H13 H 0.1381 0.2580 0.2076 0.029 Uiso 1 1 calc R . .
C14 C 0.1517(5) 0.26166(15) -0.1288(4) 0.0477(10) Uani 1 1 d . . .
H14A H 0.0580 0.2649 -0.1935 0.057 Uiso 1 1 calc R . .
H14B H 0.1886 0.2225 -0.1283 0.057 Uiso 1 1 calc R . .
H14C H 0.2288 0.2870 -0.1592 0.057 Uiso 1 1 calc R . .
C15 C 0.0530(4) 0.33304(14) 0.0248(4) 0.0437(10) Uani 1 1 d . . .
H15C H -0.0486 0.3337 -0.0280 0.052 Uiso 1 1 calc R . .
H15B H 0.1163 0.3621 -0.0120 0.052 Uiso 1 1 calc R . .
H15A H 0.0451 0.3407 0.1237 0.052 Uiso 1 1 calc R . .
C16 C 0.3619(3) 0.04618(12) 0.4153(3) 0.0260(7) Uani 1 1 d . . .
H16 H 0.2686 0.0288 0.3796 0.031 Uiso 1 1 calc R . .
C17 C 0.6045(4) 0.03981(15) 0.5483(5) 0.0613(14) Uani 1 1 d . . .
H17A H 0.6034 0.0446 0.6492 0.074 Uiso 1 1 calc R . .
H17B H 0.6197 0.0767 0.5055 0.074 Uiso 1 1 calc R . .
H17C H 0.6873 0.0142 0.5313 0.074 Uiso 1 1 calc R . .
C18 C 0.4342(4) -0.04366(14) 0.5177(4) 0.0459(10) Uani 1 1 d . . .
H18C H 0.5172 -0.0667 0.4897 0.055 Uiso 1 1 calc R . .
H18B H 0.3380 -0.0559 0.4657 0.055 Uiso 1 1 calc R . .
H18A H 0.4293 -0.0483 0.6182 0.055 Uiso 1 1 calc R . .
N1 N 0.4895(3) 0.26039(10) 0.5244(3) 0.0238(6) Uani 1 1 d . . .
N2 N -0.0492(3) 0.16005(13) 0.5007(3) 0.0384(7) Uani 1 1 d . . .
N3 N 0.0941(3) 0.02618(11) -0.0161(3) 0.0333(6) Uani 1 1 d . . .
N4 N 0.6583(3) 0.15792(12) 0.0443(3) 0.0359(7) Uani 1 1 d . . .
N5 N 0.1216(3) 0.27734(10) 0.0109(3) 0.0264(6) Uani 1 1 d . . .
N6 N 0.4610(3) 0.01602(11) 0.4874(3) 0.0297(7) Uani 1 1 d . . .
N37 N -0.5168(3) -0.09798(12) -1.0125(3) 0.0385(7) Uani 1 1 d . . .
O21 O -0.5166(4) -0.19281(13) -1.0405(4) 0.0748(10) Uani 1 1 d . . .
C21 C -0.4746(5) -0.14568(17) -1.0684(5) 0.0522(11) Uani 1 1 d . . .
H21 H -0.4056 -0.1428 -1.1362 0.063 Uiso 1 1 calc R . .
C22 C -0.4540(5) -0.04441(17) -1.0468(5) 0.0624(12) Uani 1 1 d . . .
H22A H -0.5345 -0.0204 -1.0942 0.075 Uiso 1 1 calc R . .
H22B H -0.3756 -0.0506 -1.1088 0.075 Uiso 1 1 calc R . .
H22C H -0.4089 -0.0257 -0.9610 0.075 Uiso 1 1 calc R . .
C23 C -0.6204(4) -0.0985(2) -0.9112(5) 0.0586(11) Uani 1 1 d . . .
H23C H -0.5752 -0.0789 -0.8266 0.070 Uiso 1 1 calc R . .
H23B H -0.6434 -0.1378 -0.8882 0.070 Uiso 1 1 calc R . .
H23A H -0.7143 -0.0792 -0.9489 0.070 Uiso 1 1 calc R . .
Cl11 Cl 0.36648(12) 0.12485(4) -0.23800(9) 0.0478(2) Uani 1 1 d . . .


_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
Tc1 Cl6 2.3523(7) . ?
Tc1 Cl3 2.3531(7) . ?
Tc1 Cl4 2.3549(8) . ?
Tc1 Cl5 2.3577(7) . ?
Tc1 Cl2 2.3580(8) . ?
Tc1 Cl1 2.3605(8) . ?
Al1 O6 1.862(2) . ?
Al1 O1 1.872(2) . ?
Al1 O5 1.875(2) . ?
Al1 O3 1.881(2) . ?
Al1 O2 1.890(2) . ?
Al1 O4 1.892(2) . ?
O1 C1 1.265(3) . ?
O2 C4 1.257(4) . ?
O3 C7 1.248(4) . ?
O4 C10 1.256(4) . ?
O5 C13 1.272(3) . ?
O6 C16 1.261(3) . ?
C1 N1 1.304(4) . ?
C1 H1 0.9500 . ?
C2 N1 1.458(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 N1 1.448(4) . ?
C3 H3C 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3A 0.9800 . ?
C4 N2 1.299(4) . ?
C4 H4 0.9500 . ?
C5 N2 1.437(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N2 1.445(5) . ?
C6 H6C 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6A 0.9800 . ?
C7 N3 1.308(4) . ?
C7 H7 0.9500 . ?
C8 N3 1.459(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N3 1.457(5) . ?
C9 H9C 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9A 0.9800 . ?
C10 N4 1.297(4) . ?
C10 H10 0.9500 . ?
C11 N4 1.443(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N4 1.449(5) . ?
C12 H12C 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12A 0.9800 . ?
C13 N5 1.291(4) . ?
C13 H13 0.9500 . ?
C14 N5 1.451(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N5 1.462(4) . ?
C15 H15C 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15A 0.9800 . ?
C16 N6 1.271(4) . ?
C16 H16 0.9500 . ?
C17 N6 1.449(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 N6 1.464(4) . ?
C18 H18C 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18A 0.9800 . ?
N37 C21 1.321(5) . ?
N37 C23 1.419(4) . ?
N37 C22 1.436(5) . ?
O21 C21 1.213(5) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23C 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23A 0.9800 . ?

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
Cl6 Tc1 Cl3 89.64(3) . . ?
Cl6 Tc1 Cl4 89.78(3) . . ?
Cl3 Tc1 Cl4 90.04(3) . . ?
Cl6 Tc1 Cl5 179.49(3) . . ?
Cl3 Tc1 Cl5 89.88(3) . . ?
Cl4 Tc1 Cl5 90.06(3) . . ?
Cl6 Tc1 Cl2 88.48(3) . . ?
Cl3 Tc1 Cl2 89.65(3) . . ?
Cl4 Tc1 Cl2 178.23(3) . . ?
Cl5 Tc1 Cl2 91.68(3) . . ?
Cl6 Tc1 Cl1 91.80(3) . . ?
Cl3 Tc1 Cl1 178.18(3) . . ?
Cl4 Tc1 Cl1 91.08(3) . . ?
Cl5 Tc1 Cl1 88.68(3) . . ?
Cl2 Tc1 Cl1 89.28(3) . . ?
O6 Al1 O1 88.90(9) . . ?
O6 Al1 O5 176.26(11) . . ?
O1 Al1 O5 89.36(9) . . ?
O6 Al1 O3 90.89(9) . . ?
O1 Al1 O3 179.22(11) . . ?
O5 Al1 O3 90.90(10) . . ?
O6 Al1 O2 94.26(10) . . ?
O1 Al1 O2 92.83(9) . . ?
O5 Al1 O2 89.13(10) . . ?
O3 Al1 O2 86.44(10) . . ?
O6 Al1 O4 87.79(10) . . ?
O1 Al1 O4 90.18(10) . . ?
O5 Al1 O4 88.92(10) . . ?
O3 Al1 O4 90.56(10) . . ?
O2 Al1 O4 176.39(11) . . ?
C1 O1 Al1 128.72(19) . . ?
C4 O2 Al1 133.1(2) . . ?
C7 O3 Al1 129.5(2) . . ?
C10 O4 Al1 127.5(2) . . ?
C13 O5 Al1 128.6(2) . . ?
C16 O6 Al1 132.5(2) . . ?
O1 C1 N1 122.6(3) . . ?
O1 C1 H1 118.7 . . ?
N1 C1 H1 118.7 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3C 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3C C3 H3B 109.5 . . ?
N1 C3 H3A 109.5 . . ?
H3C C3 H3A 109.5 . . ?
H3B C3 H3A 109.5 . . ?
O2 C4 N2 122.4(3) . . ?
O2 C4 H4 118.8 . . ?
N2 C4 H4 118.8 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6C 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6C C6 H6B 109.5 . . ?
N2 C6 H6A 109.5 . . ?
H6C C6 H6A 109.5 . . ?
H6B C6 H6A 109.5 . . ?
O3 C7 N3 122.0(3) . . ?
O3 C7 H7 119.0 . . ?
N3 C7 H7 119.0 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 H9C 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9C C9 H9B 109.5 . . ?
N3 C9 H9A 109.5 . . ?
H9C C9 H9A 109.5 . . ?
H9B C9 H9A 109.5 . . ?
O4 C10 N4 123.1(3) . . ?
O4 C10 H10 118.5 . . ?
N4 C10 H10 118.5 . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 H12C 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12C C12 H12B 109.5 . . ?
N4 C12 H12A 109.5 . . ?
H12C C12 H12A 109.5 . . ?
H12B C12 H12A 109.5 . . ?
O5 C13 N5 122.4(3) . . ?
O5 C13 H13 118.8 . . ?
N5 C13 H13 118.8 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N5 C15 H15C 109.5 . . ?
N5 C15 H15B 109.5 . . ?
H15C C15 H15B 109.5 . . ?
N5 C15 H15A 109.5 . . ?
H15C C15 H15A 109.5 . . ?
H15B C15 H15A 109.5 . . ?
O6 C16 N6 123.7(3) . . ?
O6 C16 H16 118.1 . . ?
N6 C16 H16 118.1 . . ?
N6 C17 H17A 109.5 . . ?
N6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N6 C18 H18C 109.5 . . ?
N6 C18 H18B 109.5 . . ?
H18C C18 H18B 109.5 . . ?
N6 C18 H18A 109.5 . . ?
H18C C18 H18A 109.5 . . ?
H18B C18 H18A 109.5 . . ?
C1 N1 C3 121.5(3) . . ?
C1 N1 C2 120.8(3) . . ?
C3 N1 C2 117.3(3) . . ?
C4 N2 C5 122.6(3) . . ?
C4 N2 C6 119.4(3) . . ?
C5 N2 C6 117.7(4) . . ?
C7 N3 C9 120.9(3) . . ?
C7 N3 C8 121.5(3) . . ?
C9 N3 C8 117.6(3) . . ?
C10 N4 C11 120.6(3) . . ?
C10 N4 C12 121.6(3) . . ?
C11 N4 C12 117.5(3) . . ?
C13 N5 C14 122.5(3) . . ?
C13 N5 C15 121.5(3) . . ?
C14 N5 C15 116.0(3) . . ?
C16 N6 C17 121.4(3) . . ?
C16 N6 C18 122.0(3) . . ?
C17 N6 C18 116.6(3) . . ?
C21 N37 C23 120.8(3) . . ?
C21 N37 C22 121.3(3) . . ?
C23 N37 C22 117.9(4) . . ?
O21 C21 N37 125.5(4) . . ?
O21 C21 H21 117.2 . . ?
N37 C21 H21 117.2 . . ?
N37 C22 H22A 109.5 . . ?
N37 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N37 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N37 C23 H23C 109.5 . . ?
N37 C23 H23B 109.5 . . ?
H23C C23 H23B 109.5 . . ?
N37 C23 H23A 109.5 . . ?
H23C C23 H23A 109.5 . . ?
H23B C23 H23A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Al1 O1 C1 -34.8(2) . . . . ?
O5 Al1 O1 C1 148.5(2) . . . . ?
O3 Al1 O1 C1 40(8) . . . . ?
O2 Al1 O1 C1 59.4(2) . . . . ?
O4 Al1 O1 C1 -122.6(2) . . . . ?
O6 Al1 O2 C4 16.8(3) . . . . ?
O1 Al1 O2 C4 -72.4(3) . . . . ?
O5 Al1 O2 C4 -161.7(3) . . . . ?
O3 Al1 O2 C4 107.4(3) . . . . ?
O4 Al1 O2 C4 141.2(15) . . . . ?
O6 Al1 O3 C7 -129.7(3) . . . . ?
O1 Al1 O3 C7 156(8) . . . . ?
O5 Al1 O3 C7 47.0(3) . . . . ?
O2 Al1 O3 C7 136.1(3) . . . . ?
O4 Al1 O3 C7 -41.9(3) . . . . ?
O6 Al1 O4 C10 -133.9(3) . . . . ?
O1 Al1 O4 C10 -45.0(3) . . . . ?
O5 Al1 O4 C10 44.4(3) . . . . ?
O3 Al1 O4 C10 135.2(3) . . . . ?
O2 Al1 O4 C10 101.5(16) . . . . ?
O6 Al1 O5 C13 -104.0(16) . . . . ?
O1 Al1 O5 C13 -41.9(2) . . . . ?
O3 Al1 O5 C13 137.4(2) . . . . ?
O2 Al1 O5 C13 51.0(2) . . . . ?
O4 Al1 O5 C13 -132.1(2) . . . . ?
O1 Al1 O6 C16 171.5(3) . . . . ?
O5 Al1 O6 C16 -126.4(15) . . . . ?
O3 Al1 O6 C16 -7.8(3) . . . . ?
O2 Al1 O6 C16 78.7(3) . . . . ?
O4 Al1 O6 C16 -98.3(3) . . . . ?
Al1 O1 C1 N1 -178.1(2) . . . . ?
Al1 O2 C4 N2 179.2(2) . . . . ?
Al1 O3 C7 N3 -177.7(2) . . . . ?
Al1 O4 C10 N4 169.2(2) . . . . ?
Al1 O5 C13 N5 170.2(2) . . . . ?
Al1 O6 C16 N6 158.9(3) . . . . ?
O1 C1 N1 C3 174.1(3) . . . . ?
O1 C1 N1 C2 2.0(5) . . . . ?
O2 C4 N2 C5 -3.2(6) . . . . ?
O2 C4 N2 C6 -176.7(3) . . . . ?
O3 C7 N3 C9 -179.8(3) . . . . ?
O3 C7 N3 C8 0.7(5) . . . . ?
O4 C10 N4 C11 3.8(6) . . . . ?
O4 C10 N4 C12 177.5(4) . . . . ?
O5 C13 N5 C14 -3.9(5) . . . . ?
O5 C13 N5 C15 176.7(3) . . . . ?
O6 C16 N6 C17 1.6(5) . . . . ?
O6 C16 N6 C18 179.1(3) . . . . ?
C23 N37 C21 O21 -0.4(7) . . . . ?
C22 N37 C21 O21 176.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 1017769'
