# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sj041115
_database_code_depnum_ccdc_archive 'CCDC 1554161'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Tc(Me6Ph)2](PF6)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H36 F6 P Tc'
_chemical_formula_sum            'C24 H36 F6 P Tc'
_chemical_formula_weight         567.50

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   'P n n m'

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

_cell_length_a                   8.1154(6)
_cell_length_b                   10.4942(6)
_cell_length_c                   13.6880(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1165.73(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    2219
_cell_measurement_theta_min      2.9200
_cell_measurement_theta_max      31.1170

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9140
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            7912
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         30.49
_reflns_number_total             1853
_reflns_number_gt                1390
_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)+(0.0310P)²+0.1180P] 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         1853
_refine_ls_number_parameters     81
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0846
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_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 1.0000 0.0000 0.5000 0.01563(11) Uani 1 4 d S . .
C1 C 0.8803(3) 0.1826(2) 0.44802(16) 0.0267(5) Uani 1 1 d . . .
C2 C 0.8103(3) 0.0791(2) 0.39662(15) 0.0256(5) Uani 1 1 d . . .
C3 C 0.7390(3) -0.0255(2) 0.44807(16) 0.0241(5) Uani 1 1 d . . .
C4 C 0.9500(4) 0.2968(3) 0.3941(2) 0.0481(8) Uani 1 1 d . . .
H4A H 0.9779 0.2722 0.3271 0.058 Uiso 1 1 calc R . .
H4B H 1.0494 0.3269 0.4276 0.058 Uiso 1 1 calc R . .
H4C H 0.8677 0.3652 0.3928 0.058 Uiso 1 1 calc R . .
C5 C 0.8029(4) 0.0802(3) 0.28589(17) 0.0540(9) Uani 1 1 d . . .
H5A H 0.7905 -0.0072 0.2618 0.065 Uiso 1 1 calc R . .
H5B H 0.9048 0.1171 0.2598 0.065 Uiso 1 1 calc R . .
H5C H 0.7087 0.1315 0.2645 0.065 Uiso 1 1 calc R . .
C6 C 0.6596(4) -0.1335(2) 0.3932(2) 0.0465(8) Uani 1 1 d . . .
H6A H 0.6852 -0.2142 0.4258 0.056 Uiso 1 1 calc R . .
H6B H 0.7019 -0.1355 0.3262 0.056 Uiso 1 1 calc R . .
H6C H 0.5399 -0.1211 0.3919 0.056 Uiso 1 1 calc R . .
P1 P 0.5000 -0.5000 0.5000 0.0290(3) Uani 1 4 d S . .
F1 F 0.4489(2) -0.39983(16) 0.58203(12) 0.0536(5) Uani 1 1 d . . .
F2 F 0.6833(3) -0.4440(2) 0.5000 0.0507(6) Uani 1 2 d S . .


_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 C2 2.250(2) 5_756 ?
Tc1 C2 2.250(2) 6_556 ?
Tc1 C2 2.250(2) . ?
Tc1 C2 2.250(2) 2_755 ?
Tc1 C3 2.250(2) 5_756 ?
Tc1 C3 2.250(2) 6_556 ?
Tc1 C3 2.250(2) . ?
Tc1 C3 2.250(2) 2_755 ?
Tc1 C1 2.263(2) 2_755 ?
Tc1 C1 2.263(2) 5_756 ?
Tc1 C1 2.263(2) . ?
Tc1 C1 2.263(2) 6_556 ?
C1 C2 1.413(3) . ?
C1 C1 1.423(4) 6_556 ?
C1 C4 1.517(3) . ?
C2 C3 1.428(3) . ?
C2 C5 1.517(3) . ?
C3 C3 1.422(4) 6_556 ?
C3 C6 1.504(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
P1 F1 1.5929(16) 2_645 ?
P1 F1 1.5929(16) 5_646 ?
P1 F1 1.5929(16) 6_556 ?
P1 F1 1.5930(16) . ?
P1 F2 1.599(2) . ?
P1 F2 1.599(2) 5_646 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Tc1 C2 102.05(11) 5_756 6_556 ?
C2 Tc1 C2 180.00(9) 5_756 . ?
C2 Tc1 C2 77.95(11) 6_556 . ?
C2 Tc1 C2 77.95(11) 5_756 2_755 ?
C2 Tc1 C2 180.0 6_556 2_755 ?
C2 Tc1 C2 102.05(11) . 2_755 ?
C2 Tc1 C3 36.99(8) 5_756 5_756 ?
C2 Tc1 C3 113.66(8) 6_556 5_756 ?
C2 Tc1 C3 143.01(8) . 5_756 ?
C2 Tc1 C3 66.34(8) 2_755 5_756 ?
C2 Tc1 C3 113.66(8) 5_756 6_556 ?
C2 Tc1 C3 36.99(8) 6_556 6_556 ?
C2 Tc1 C3 66.34(8) . 6_556 ?
C2 Tc1 C3 143.01(8) 2_755 6_556 ?
C3 Tc1 C3 143.17(12) 5_756 6_556 ?
C2 Tc1 C3 143.01(8) 5_756 . ?
C2 Tc1 C3 66.34(8) 6_556 . ?
C2 Tc1 C3 36.99(8) . . ?
C2 Tc1 C3 113.66(8) 2_755 . ?
C3 Tc1 C3 179.999(1) 5_756 . ?
C3 Tc1 C3 36.83(12) 6_556 . ?
C2 Tc1 C3 66.34(8) 5_756 2_755 ?
C2 Tc1 C3 143.01(8) 6_556 2_755 ?
C2 Tc1 C3 113.66(8) . 2_755 ?
C2 Tc1 C3 36.99(8) 2_755 2_755 ?
C3 Tc1 C3 36.83(12) 5_756 2_755 ?
C3 Tc1 C3 179.999(1) 6_556 2_755 ?
C3 Tc1 C3 143.17(12) . 2_755 ?
C2 Tc1 C1 65.89(8) 5_756 2_755 ?
C2 Tc1 C1 143.51(8) 6_556 2_755 ?
C2 Tc1 C1 114.10(8) . 2_755 ?
C2 Tc1 C1 36.49(8) 2_755 2_755 ?
C3 Tc1 C1 78.24(8) 5_756 2_755 ?
C3 Tc1 C1 113.73(8) 6_556 2_755 ?
C3 Tc1 C1 101.76(8) . 2_755 ?
C3 Tc1 C1 66.27(8) 2_755 2_755 ?
C2 Tc1 C1 36.49(8) 5_756 5_756 ?
C2 Tc1 C1 114.10(8) 6_556 5_756 ?
C2 Tc1 C1 143.51(8) . 5_756 ?
C2 Tc1 C1 65.90(8) 2_755 5_756 ?
C3 Tc1 C1 66.27(8) 5_756 5_756 ?
C3 Tc1 C1 101.76(8) 6_556 5_756 ?
C3 Tc1 C1 113.73(8) . 5_756 ?
C3 Tc1 C1 78.24(8) 2_755 5_756 ?
C1 Tc1 C1 36.66(11) 2_755 5_756 ?
C2 Tc1 C1 143.51(8) 5_756 . ?
C2 Tc1 C1 65.89(8) 6_556 . ?
C2 Tc1 C1 36.49(8) . . ?
C2 Tc1 C1 114.11(8) 2_755 . ?
C3 Tc1 C1 113.73(8) 5_756 . ?
C3 Tc1 C1 78.24(8) 6_556 . ?
C3 Tc1 C1 66.27(8) . . ?
C3 Tc1 C1 101.76(8) 2_755 . ?
C1 Tc1 C1 143.35(11) 2_755 . ?
C1 Tc1 C1 180.0 5_756 . ?
C2 Tc1 C1 114.11(8) 5_756 6_556 ?
C2 Tc1 C1 36.49(8) 6_556 6_556 ?
C2 Tc1 C1 65.90(8) . 6_556 ?
C2 Tc1 C1 143.51(8) 2_755 6_556 ?
C3 Tc1 C1 101.76(8) 5_756 6_556 ?
C3 Tc1 C1 66.26(8) 6_556 6_556 ?
C3 Tc1 C1 78.24(8) . 6_556 ?
C3 Tc1 C1 113.74(8) 2_755 6_556 ?
C1 Tc1 C1 180.0 2_755 6_556 ?
C1 Tc1 C1 143.34(11) 5_756 6_556 ?
C1 Tc1 C1 36.66(11) . 6_556 ?
C2 C1 C1 119.87(12) . 6_556 ?
C2 C1 C4 121.0(2) . . ?
C1 C1 C4 119.10(15) 6_556 . ?
C2 C1 Tc1 71.25(12) . . ?
C1 C1 Tc1 71.67(5) 6_556 . ?
C4 C1 Tc1 131.47(18) . . ?
C1 C2 C3 120.58(18) . . ?
C1 C2 C5 120.5(2) . . ?
C3 C2 C5 118.9(2) . . ?
C1 C2 Tc1 72.26(13) . . ?
C3 C2 Tc1 71.53(12) . . ?
C5 C2 Tc1 131.18(18) . . ?
C3 C3 C2 119.56(12) 6_556 . ?
C3 C3 C6 119.95(14) 6_556 . ?
C2 C3 C6 120.5(2) . . ?
C3 C3 Tc1 71.59(6) 6_556 . ?
C2 C3 Tc1 71.48(13) . . ?
C6 C3 Tc1 130.58(17) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
F1 P1 F1 89.64(13) 2_645 5_646 ?
F1 P1 F1 180.0 2_645 6_556 ?
F1 P1 F1 90.36(13) 5_646 6_556 ?
F1 P1 F1 90.36(13) 2_645 . ?
F1 P1 F1 180.0 5_646 . ?
F1 P1 F1 89.64(13) 6_556 . ?
F1 P1 F2 90.03(9) 2_645 . ?
F1 P1 F2 90.03(9) 5_646 . ?
F1 P1 F2 89.97(9) 6_556 . ?
F1 P1 F2 89.97(9) . . ?
F1 P1 F2 89.97(9) 2_645 5_646 ?
F1 P1 F2 89.97(9) 5_646 5_646 ?
F1 P1 F2 90.03(9) 6_556 5_646 ?
F1 P1 F2 90.03(9) . 5_646 ?
F2 P1 F2 180.0 . 5_646 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Tc1 C1 C2 180.0 5_756 . . . ?
C2 Tc1 C1 C2 -102.73(18) 6_556 . . . ?
C2 Tc1 C1 C2 77.26(18) 2_755 . . . ?
C3 Tc1 C1 C2 150.79(13) 5_756 . . . ?
C3 Tc1 C1 C2 -65.93(14) 6_556 . . . ?
C3 Tc1 C1 C2 -29.21(13) . . . . ?
C3 Tc1 C1 C2 114.07(14) 2_755 . . . ?
C1 Tc1 C1 C2 48.21(12) 2_755 . . . ?
C1 Tc1 C1 C2 -115(6) 5_756 . . . ?
C1 Tc1 C1 C2 -131.79(12) 6_556 . . . ?
C2 Tc1 C1 C1 -48.21(11) 5_756 . . 6_556 ?
C2 Tc1 C1 C1 29.06(8) 6_556 . . 6_556 ?
C2 Tc1 C1 C1 131.79(11) . . . 6_556 ?
C2 Tc1 C1 C1 -150.94(8) 2_755 . . 6_556 ?
C3 Tc1 C1 C1 -77.42(7) 5_756 . . 6_556 ?
C3 Tc1 C1 C1 65.87(6) 6_556 . . 6_556 ?
C3 Tc1 C1 C1 102.58(7) . . . 6_556 ?
C3 Tc1 C1 C1 -114.14(6) 2_755 . . 6_556 ?
C1 Tc1 C1 C1 179.998(1) 2_755 . . 6_556 ?
C1 Tc1 C1 C1 17(6) 5_756 . . 6_556 ?
C2 Tc1 C1 C4 64.8(3) 5_756 . . . ?
C2 Tc1 C1 C4 142.1(3) 6_556 . . . ?
C2 Tc1 C1 C4 -115.2(3) . . . . ?
C2 Tc1 C1 C4 -37.9(3) 2_755 . . . ?
C3 Tc1 C1 C4 35.6(3) 5_756 . . . ?
C3 Tc1 C1 C4 178.9(2) 6_556 . . . ?
C3 Tc1 C1 C4 -144.4(3) . . . . ?
C3 Tc1 C1 C4 -1.1(2) 2_755 . . . ?
C1 Tc1 C1 C4 -67.0(2) 2_755 . . . ?
C1 Tc1 C1 C4 130(6) 5_756 . . . ?
C1 Tc1 C1 C4 113.0(2) 6_556 . . . ?
C1 C1 C2 C3 0.2(3) 6_556 . . . ?
C4 C1 C2 C3 -177.4(2) . . . . ?
Tc1 C1 C2 C3 54.9(2) . . . . ?
C1 C1 C2 C5 177.43(18) 6_556 . . . ?
C4 C1 C2 C5 -0.1(4) . . . . ?
Tc1 C1 C2 C5 -127.9(2) . . . . ?
C1 C1 C2 Tc1 -54.70(9) 6_556 . . . ?
C4 C1 C2 Tc1 127.7(2) . . . . ?
C2 Tc1 C2 C1 -176.7(9) 5_756 . . . ?
C2 Tc1 C2 C1 65.56(15) 6_556 . . . ?
C2 Tc1 C2 C1 -114.44(15) 2_755 . . . ?
C3 Tc1 C2 C1 -47.94(19) 5_756 . . . ?
C3 Tc1 C2 C1 102.60(14) 6_556 . . . ?
C3 Tc1 C2 C1 132.06(19) . . . . ?
C3 Tc1 C2 C1 -77.40(14) 2_755 . . . ?
C1 Tc1 C2 C1 -150.82(11) 2_755 . . . ?
C1 Tc1 C2 C1 180.0 5_756 . . . ?
C1 Tc1 C2 C1 29.18(11) 6_556 . . . ?
C2 Tc1 C2 C3 51.3(9) 5_756 . . . ?
C2 Tc1 C2 C3 -66.50(14) 6_556 . . . ?
C2 Tc1 C2 C3 113.50(14) 2_755 . . . ?
C3 Tc1 C2 C3 180.0 5_756 . . . ?
C3 Tc1 C2 C3 -29.46(12) 6_556 . . . ?
C3 Tc1 C2 C3 150.54(12) 2_755 . . . ?
C1 Tc1 C2 C3 77.12(15) 2_755 . . . ?
C1 Tc1 C2 C3 47.94(19) 5_756 . . . ?
C1 Tc1 C2 C3 -132.06(19) . . . . ?
C1 Tc1 C2 C3 -102.87(15) 6_556 . . . ?
C2 Tc1 C2 C5 -61.3(14) 5_756 . . . ?
C2 Tc1 C2 C5 -179.1(2) 6_556 . . . ?
C2 Tc1 C2 C5 0.9(2) 2_755 . . . ?
C3 Tc1 C2 C5 67.4(3) 5_756 . . . ?
C3 Tc1 C2 C5 -142.0(3) 6_556 . . . ?
C3 Tc1 C2 C5 -112.6(3) . . . . ?
C3 Tc1 C2 C5 38.0(3) 2_755 . . . ?
C1 Tc1 C2 C5 -35.4(3) 2_755 . . . ?
C1 Tc1 C2 C5 -64.6(3) 5_756 . . . ?
C1 Tc1 C2 C5 115.4(3) . . . . ?
C1 Tc1 C2 C5 144.6(3) 6_556 . . . ?
C1 C2 C3 C3 -0.2(3) . . . 6_556 ?
C5 C2 C3 C3 -177.48(17) . . . 6_556 ?
Tc1 C2 C3 C3 55.04(9) . . . 6_556 ?
C1 C2 C3 C6 178.0(2) . . . . ?
C5 C2 C3 C6 0.7(4) . . . . ?
Tc1 C2 C3 C6 -126.8(2) . . . . ?
C1 C2 C3 Tc1 -55.2(2) . . . . ?
C5 C2 C3 Tc1 127.5(2) . . . . ?
C2 Tc1 C3 C3 48.71(11) 5_756 . . 6_556 ?
C2 Tc1 C3 C3 -29.58(8) 6_556 . . 6_556 ?
C2 Tc1 C3 C3 -131.29(11) . . . 6_556 ?
C2 Tc1 C3 C3 150.42(8) 2_755 . . 6_556 ?
C3 Tc1 C3 C3 141.2(10) 5_756 . . 6_556 ?
C3 Tc1 C3 C3 180.0 2_755 . . 6_556 ?
C1 Tc1 C3 C3 114.07(6) 2_755 . . 6_556 ?
C1 Tc1 C3 C3 77.55(7) 5_756 . . 6_556 ?
C1 Tc1 C3 C3 -102.45(7) . . . 6_556 ?
C1 Tc1 C3 C3 -65.93(6) 6_556 . . 6_556 ?
C2 Tc1 C3 C2 180.0 5_756 . . . ?
C2 Tc1 C3 C2 101.71(18) 6_556 . . . ?
C2 Tc1 C3 C2 -78.29(18) 2_755 . . . ?
C3 Tc1 C3 C2 -87.5(10) 5_756 . . . ?
C3 Tc1 C3 C2 131.29(11) 6_556 . . . ?
C3 Tc1 C3 C2 -48.71(12) 2_755 . . . ?
C1 Tc1 C3 C2 -114.64(14) 2_755 . . . ?
C1 Tc1 C3 C2 -151.17(12) 5_756 . . . ?
C1 Tc1 C3 C2 28.84(12) . . . . ?
C1 Tc1 C3 C2 65.36(14) 6_556 . . . ?
C2 Tc1 C3 C6 -65.3(3) 5_756 . . . ?
C2 Tc1 C3 C6 -143.6(2) 6_556 . . . ?
C2 Tc1 C3 C6 114.7(3) . . . . ?
C2 Tc1 C3 C6 36.4(2) 2_755 . . . ?
C3 Tc1 C3 C6 27.2(11) 5_756 . . . ?
C3 Tc1 C3 C6 -114.1(2) 6_556 . . . ?
C3 Tc1 C3 C6 65.9(2) 2_755 . . . ?
C1 Tc1 C3 C6 0.0(2) 2_755 . . . ?
C1 Tc1 C3 C6 -36.5(2) 5_756 . . . ?
C1 Tc1 C3 C6 143.5(2) . . . . ?
C1 Tc1 C3 C6 -180.0(2) 6_556 . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.49
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.092
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_GIM020617_Cu
_database_code_depnum_ccdc_archive 'CCDC 1554399'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H50 F3 O12 P3 Re S'
_chemical_formula_weight         910.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.22709(11)
_cell_length_b                   15.78790(12)
_cell_length_c                   30.1873(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.4536(8)
_cell_angle_gamma                90
_cell_volume                     7579.73(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    30569
_cell_measurement_theta_min      3.1690
_cell_measurement_theta_max      78.5890

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_F_000             3672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    8.574
_shelx_estimated_absorpt_T_min   0.426
_shelx_estimated_absorpt_T_max   0.725
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.458
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27e (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41327
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.173
_diffrn_reflns_theta_max         78.974
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8073
_reflns_number_gt                7249
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.27e (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27e (Rigaku OD, 2015)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1025P)²+42.1476P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8073
_refine_ls_number_parameters     484
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1765
_refine_ls_wR_factor_gt          0.1724
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.059
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.44858(2) 0.19618(2) 0.09832(2) 0.05432(13) Uani 1 1 d . . . . .
C1 C 0.4373(5) 0.1032(5) 0.0390(3) 0.076(2) Uani 1 1 d . . . . .
H1 H 0.4758 0.0916 0.0198 0.091 Uiso 1 1 calc R U . . .
C2 C 0.4406(5) 0.0565(4) 0.0795(3) 0.085(3) Uani 1 1 d . . . . .
H2 H 0.4826 0.0145 0.0880 0.102 Uiso 1 1 calc R U . . .
C3 C 0.3827(5) 0.0720(5) 0.1068(3) 0.078(2) Uani 1 1 d . . . . .
H3 H 0.3843 0.0400 0.1336 0.093 Uiso 1 1 calc R U . . .
C4 C 0.3209(4) 0.1361(5) 0.0942(3) 0.0736(19) Uani 1 1 d . . . . .
H4 H 0.2821 0.1476 0.1133 0.088 Uiso 1 1 calc R U . . .
C5 C 0.3162(4) 0.1819(5) 0.0549(3) 0.072(2) Uani 1 1 d . . . . .
H5 H 0.2731 0.2229 0.0462 0.086 Uiso 1 1 calc R U . . .
C6 C 0.3757(5) 0.1673(5) 0.0278(3) 0.0716(19) Uani 1 1 d . . . . .
H6 H 0.3747 0.2009 0.0015 0.086 Uiso 1 1 calc R U . . .
C7 C 0.7021(7) 0.0822(8) 0.0885(4) 0.118(4) Uani 1 1 d D U . . .
H7A H 0.6909 0.0205 0.0874 0.142 Uiso 0.4 1 calc R U P A 3
H7B H 0.7374 0.0952 0.1185 0.142 Uiso 0.4 1 calc R U P A 3
H7C H 0.7089 0.0404 0.1134 0.142 Uiso 0.6 1 calc R U P B 4
H7D H 0.7499 0.1223 0.0945 0.142 Uiso 0.6 1 calc R U P B 4
C8 C 0.750(3) 0.104(5) 0.0529(17) 0.24(4) Uani 0.4 1 d D U P C 3
H8A H 0.8024 0.0716 0.0578 0.358 Uiso 0.4 1 calc R U P C 3
H8B H 0.7160 0.0899 0.0232 0.358 Uiso 0.4 1 calc R U P C 3
H8C H 0.7626 0.1647 0.0542 0.358 Uiso 0.4 1 calc R U P C 3
C8B C 0.6972(16) 0.0388(13) 0.0440(5) 0.119(7) Uani 0.6 1 d D U P C 4
H8B1 H 0.7491 0.0069 0.0444 0.178 Uiso 0.6 1 calc R U P C 4
H8B2 H 0.6492 -0.0002 0.0387 0.178 Uiso 0.6 1 calc R U P C 4
H8B3 H 0.6900 0.0812 0.0199 0.178 Uiso 0.6 1 calc R U P C 4
C9 C 0.5933(6) 0.0588(6) 0.1842(4) 0.099(3) Uani 1 1 d . . . . .
H9A H 0.6042 0.0075 0.1674 0.119 Uiso 1 1 calc R U . . .
H9B H 0.5316 0.0670 0.1795 0.119 Uiso 1 1 calc R U . . .
C10 C 0.6284(9) 0.0474(11) 0.2328(5) 0.150(6) Uani 1 1 d . . . . .
H10A H 0.6023 -0.0021 0.2441 0.225 Uiso 1 1 calc R U . . .
H10B H 0.6893 0.0386 0.2373 0.225 Uiso 1 1 calc R U . . .
H10C H 0.6169 0.0980 0.2494 0.225 Uiso 1 1 calc R U . . .
C11 C 0.7344(12) 0.2627(11) 0.1512(6) 0.077(4) Uiso 0.5 1 d D . P D 7
H11A H 0.7710 0.2304 0.1347 0.092 Uiso 0.5 1 calc R U P D 7
H11B H 0.7389 0.2372 0.1816 0.092 Uiso 0.5 1 calc R U P D 7
C12 C 0.761(2) 0.3535(14) 0.1555(11) 0.131(10) Uiso 0.5 1 d D . P D 7
H12A H 0.8197 0.3570 0.1719 0.197 Uiso 0.5 1 calc R U P D 7
H12B H 0.7569 0.3781 0.1253 0.197 Uiso 0.5 1 calc R U P D 7
H12C H 0.7250 0.3849 0.1720 0.197 Uiso 0.5 1 calc R U P D 7
C11B C 0.710(2) 0.290(2) 0.1608(12) 0.138(11) Uiso 0.5 1 d D . P D 8
H11C H 0.7380 0.2424 0.1793 0.166 Uiso 0.5 1 calc R U P D 8
H11D H 0.6838 0.3271 0.1805 0.166 Uiso 0.5 1 calc R U P D 8
C12B C 0.7744(13) 0.3402(14) 0.1398(8) 0.087(5) Uiso 0.5 1 d D . P D 8
H12D H 0.8183 0.3627 0.1640 0.130 Uiso 0.5 1 calc R U P D 8
H12E H 0.8000 0.3027 0.1205 0.130 Uiso 0.5 1 calc R U P D 8
H12F H 0.7460 0.3871 0.1217 0.130 Uiso 0.5 1 calc R U P D 8
C13 C 0.3738(10) 0.1829(9) 0.2373(5) 0.125(5) Uani 1 1 d . . . . .
H13A H 0.3544 0.2417 0.2400 0.150 Uiso 1 1 calc R U . . .
H13B H 0.4193 0.1706 0.2636 0.150 Uiso 1 1 calc R U . . .
C14 C 0.3043(13) 0.1240(14) 0.2363(6) 0.203(9) Uani 1 1 d . . . . .
H14C H 0.2824 0.1298 0.2641 0.305 Uiso 1 1 calc R U . . .
H14B H 0.2595 0.1368 0.2102 0.305 Uiso 1 1 calc R U . . .
H14A H 0.3241 0.0659 0.2337 0.305 Uiso 1 1 calc R U . . .
C15 C 0.5374(9) 0.3250(12) 0.2388(5) 0.151(6) Uani 1 1 d . . . . .
H15 H 0.4919 0.3374 0.2532 0.181 Uiso 1 1 calc R U . . .
C16 C 0.6195(11) 0.3557(12) 0.2567(4) 0.163(7) Uani 1 1 d . . . . .
H16C H 0.6187 0.3886 0.2841 0.245 Uiso 1 1 calc R U . . .
H16B H 0.6582 0.3078 0.2640 0.245 Uiso 1 1 calc R U . . .
H16A H 0.6383 0.3919 0.2343 0.245 Uiso 1 1 calc R U . . .
C17 C 0.3006(5) 0.3394(6) 0.1464(3) 0.077(2) Uani 1 1 d . . . . .
H17A H 0.3023 0.3262 0.1145 0.093 Uiso 1 1 calc R U . . .
H17B H 0.2588 0.3016 0.1562 0.093 Uiso 1 1 calc R U . . .
C18 C 0.2773(7) 0.4270(7) 0.1506(3) 0.102(3) Uani 1 1 d . . . . .
H18A H 0.2218 0.4374 0.1317 0.153 Uiso 1 1 calc R U . . .
H18B H 0.2756 0.4393 0.1822 0.153 Uiso 1 1 calc R U . . .
H18C H 0.3189 0.4638 0.1407 0.153 Uiso 1 1 calc R U . . .
C19 C 0.5525(8) 0.4483(9) 0.1303(5) 0.065(3) Uani 0.5 1 d D U P E 5
H19A H 0.5929 0.4586 0.1103 0.078 Uiso 0.5 1 calc R U P E 5
H19B H 0.5803 0.4156 0.1571 0.078 Uiso 0.5 1 calc R U P E 5
C20 C 0.5134(18) 0.5336(17) 0.1441(16) 0.167(18) Uani 0.5 1 d D U P E 5
H20A H 0.5582 0.5694 0.1609 0.250 Uiso 0.5 1 calc R U P E 5
H20B H 0.4851 0.5634 0.1168 0.250 Uiso 0.5 1 calc R U P E 5
H20C H 0.4726 0.5209 0.1632 0.250 Uiso 0.5 1 calc R U P E 5
C19B C 0.5291(14) 0.4820(12) 0.1098(7) 0.099(6) Uiso 0.5 1 d D . P E 6
H19C H 0.5028 0.5215 0.0856 0.119 Uiso 0.5 1 calc R U P E 6
H19D H 0.5856 0.4672 0.1045 0.119 Uiso 0.5 1 calc R U P E 6
C20B C 0.5377(18) 0.5255(18) 0.1555(8) 0.100(8) Uiso 0.5 1 d D . P E 6
H20D H 0.5722 0.5766 0.1560 0.151 Uiso 0.5 1 calc R U P E 6
H20E H 0.4819 0.5411 0.1606 0.151 Uiso 0.5 1 calc R U P E 6
H20F H 0.5647 0.4868 0.1794 0.151 Uiso 0.5 1 calc R U P E 6
C21 C 0.3829(5) 0.4404(5) 0.0141(3) 0.0713(18) Uani 1 1 d . . . . .
H21A H 0.4403 0.4625 0.0149 0.086 Uiso 1 1 calc R U . . .
H21B H 0.3523 0.4818 0.0294 0.086 Uiso 1 1 calc R U . . .
C22 C 0.3382(6) 0.4290(6) -0.0338(3) 0.082(2) Uani 1 1 d . . . . .
H22A H 0.3349 0.4835 -0.0496 0.122 Uiso 1 1 calc R U . . .
H22B H 0.3691 0.3884 -0.0489 0.122 Uiso 1 1 calc R U . . .
H22C H 0.2813 0.4076 -0.0344 0.122 Uiso 1 1 calc R U . . .
C23 C 0.5588(6) 0.2960(6) 0.0116(3) 0.080(2) Uani 1 1 d . . . . .
H23A H 0.5546 0.2359 0.0203 0.096 Uiso 1 1 calc R U . . .
H23B H 0.5162 0.3069 -0.0161 0.096 Uiso 1 1 calc R U . . .
C24 C 0.6420(7) 0.3137(7) 0.0037(4) 0.104(3) Uani 1 1 d . . . . .
H24A H 0.6534 0.2773 -0.0207 0.156 Uiso 1 1 calc R U . . .
H24B H 0.6454 0.3732 -0.0050 0.156 Uiso 1 1 calc R U . . .
H24C H 0.6836 0.3025 0.0313 0.156 Uiso 1 1 calc R U . . .
O1 O 0.6261(4) 0.1251(5) 0.0845(2) 0.103(2) Uani 1 1 d . . . . .
O2 O 0.6314(4) 0.1314(4) 0.1674(2) 0.0914(18) Uani 1 1 d . . . . .
O3 O 0.6508(4) 0.2597(4) 0.1276(2) 0.0934(19) Uani 1 1 d . . . . .
O4 O 0.4043(5) 0.1734(4) 0.1967(2) 0.0938(18) Uani 1 1 d . . . . .
O5 O 0.5256(4) 0.2785(5) 0.2011(2) 0.0867(16) Uani 1 1 d . . . . .
O6 O 0.3832(4) 0.3263(4) 0.17486(17) 0.0725(12) Uani 1 1 d . . . . .
O7 O 0.4801(4) 0.4083(3) 0.1076(2) 0.0782(14) Uani 1 1 d D U . . .
O8 O 0.3878(3) 0.3604(3) 0.03722(17) 0.0666(11) Uani 1 1 d . . . . .
O9 O 0.5446(3) 0.3511(3) 0.04792(17) 0.0657(11) Uani 1 1 d . . . . .
O31 O 0.3905(6) 0.2479(6) -0.0842(3) 0.137(3) Uani 1 1 d . . . . .
O32 O 0.3644(14) 0.189(2) -0.1567(7) 0.210(15) Uani 0.6 1 d . . P F 1
O33 O 0.404(2) 0.113(2) -0.0939(13) 0.205(15) Uani 0.6 1 d . . P F 1
C31 C 0.5157(14) 0.1910(14) -0.1237(12) 0.118(5) Uani 0.6 1 d . U P F 1
F31 F 0.5231(11) 0.1211(9) -0.1494(7) 0.127(5) Uani 0.6 1 d . U P F 1
F32 F 0.5682(12) 0.1822(13) -0.0834(9) 0.185(6) Uani 0.6 1 d . U P F 1
F33 F 0.5289(12) 0.2549(10) -0.1438(8) 0.171(5) Uani 0.6 1 d . U P F 1
S31 S 0.4162(4) 0.1904(3) -0.11538(18) 0.0745(12) Uani 0.6 1 d . U P F 1
S32 S 0.4175(5) 0.1679(5) -0.0980(3) 0.0690(16) Uani 0.4 1 d D U P F 2
C32 C 0.4851(13) 0.2043(16) -0.1254(7) 0.111(6) Uani 0.4 1 d D U P F 2
O34 O 0.481(2) 0.1282(14) -0.0610(7) 0.136(11) Uani 0.4 1 d . . P F 2
O35 O 0.372(2) 0.1129(19) -0.1261(9) 0.137(13) Uani 0.4 1 d . . P F 2
F35 F 0.5510(12) 0.2614(16) -0.1031(6) 0.129(6) Uani 0.4 1 d D U P F 2
F36 F 0.4375(19) 0.2483(15) -0.1645(7) 0.150(6) Uani 0.4 1 d D U P F 2
F34 F 0.5474(17) 0.1502(19) -0.1394(9) 0.130(6) Uani 0.4 1 d D U P F 2
P1 P 0.59130(11) 0.17857(12) 0.12160(7) 0.0651(4) Uani 1 1 d . . . . .
P2 P 0.44018(12) 0.24656(12) 0.16875(6) 0.0633(4) Uani 1 1 d . . . . .
P3 P 0.46841(9) 0.33126(10) 0.07347(6) 0.0535(3) 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
Re1 C4 2.260(7) . ?
Re1 C6 2.268(7) . ?
Re1 C3 2.272(7) . ?
Re1 C2 2.274(7) . ?
Re1 C1 2.294(7) . ?
Re1 C5 2.295(6) . ?
Re1 P2 2.2994(19) . ?
Re1 P1 2.2997(17) . ?
Re1 P3 2.3045(16) . ?
C1 C6 1.416(11) . ?
C1 C2 1.419(13) . ?
C1 H1 0.9500 . ?
C2 C3 1.388(13) . ?
C2 H2 0.9500 . ?
C3 C4 1.422(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.404(12) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 O1 1.391(11) . ?
C7 C8 1.485(19) . ?
C7 C8B 1.496(15) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 H7C 0.9900 . ?
C7 H7D 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9 O2 1.442(11) . ?
C9 C10 1.477(15) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 O3 1.402(19) . ?
C11 C12 1.497(18) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C11B O3 1.33(3) . ?
C11B C12B 1.552(18) . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13 O4 1.416(13) . ?
C13 C14 1.46(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14C 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14A 0.9800 . ?
C15 O5 1.336(15) . ?
C15 C16 1.420(18) . ?
C15 H15 0.9500 . ?
C16 H16C 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16A 0.9800 . ?
C17 C18 1.447(13) . ?
C17 O6 1.456(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 O7 1.388(12) . ?
C19 C20 1.579(17) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C19B O7 1.403(15) . ?
C19B C20B 1.525(18) . ?
C19B H19C 0.9900 . ?
C19B H19D 0.9900 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
C21 O8 1.437(8) . ?
C21 C22 1.496(11) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.444(13) . ?
C23 O9 1.453(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
O1 P1 1.594(7) . ?
O2 P1 1.591(6) . ?
O3 P1 1.592(6) . ?
O4 P2 1.607(6) . ?
O5 P2 1.609(6) . ?
O6 P2 1.594(6) . ?
O7 P3 1.581(5) . ?
O8 P3 1.598(5) . ?
O9 P3 1.612(5) . ?
O31 S32 1.428(10) . ?
O31 S31 1.429(9) . ?
O32 S31 1.360(18) . ?
O33 S31 1.42(3) . ?
C31 F33 1.22(3) . ?
C31 F32 1.35(4) . ?
C31 F31 1.37(3) . ?
C31 S31 1.68(2) . ?
S32 O35 1.33(2) . ?
S32 O34 1.49(3) . ?
S32 C32 1.604(17) . ?
C32 F34 1.45(2) . ?
C32 F36 1.453(19) . ?
C32 F35 1.457(19) . ?

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
C4 Re1 C6 64.1(3) . . ?
C4 Re1 C3 36.6(3) . . ?
C6 Re1 C3 76.3(3) . . ?
C4 Re1 C2 64.7(3) . . ?
C6 Re1 C2 65.0(3) . . ?
C3 Re1 C2 35.6(3) . . ?
C4 Re1 C1 76.0(3) . . ?
C6 Re1 C1 36.2(3) . . ?
C3 Re1 C1 64.5(3) . . ?
C2 Re1 C1 36.2(3) . . ?
C4 Re1 C5 35.3(3) . . ?
C6 Re1 C5 35.8(3) . . ?
C3 Re1 C5 64.6(3) . . ?
C2 Re1 C5 76.2(3) . . ?
C1 Re1 C5 64.6(3) . . ?
C4 Re1 P2 88.5(2) . . ?
C6 Re1 P2 145.3(2) . . ?
C3 Re1 P2 94.5(3) . . ?
C2 Re1 P2 123.7(3) . . ?
C1 Re1 P2 158.8(2) . . ?
C5 Re1 P2 110.0(2) . . ?
C4 Re1 P1 145.4(2) . . ?
C6 Re1 P1 124.6(2) . . ?
C3 Re1 P1 109.2(2) . . ?
C2 Re1 P1 87.9(2) . . ?
C1 Re1 P1 94.6(2) . . ?
C5 Re1 P1 159.1(2) . . ?
P2 Re1 P1 90.01(7) . . ?
C4 Re1 P3 123.8(2) . . ?
C6 Re1 P3 87.7(2) . . ?
C3 Re1 P3 159.2(2) . . ?
C2 Re1 P3 145.2(3) . . ?
C1 Re1 P3 109.5(2) . . ?
C5 Re1 P3 94.6(2) . . ?
P2 Re1 P3 91.07(6) . . ?
P1 Re1 P3 90.81(6) . . ?
C6 C1 C2 118.9(8) . . ?
C6 C1 Re1 70.9(4) . . ?
C2 C1 Re1 71.1(4) . . ?
C6 C1 H1 120.6 . . ?
C2 C1 H1 120.6 . . ?
Re1 C1 H1 129.7 . . ?
C3 C2 C1 120.4(7) . . ?
C3 C2 Re1 72.2(4) . . ?
C1 C2 Re1 72.7(4) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
Re1 C2 H2 127.4 . . ?
C2 C3 C4 119.4(8) . . ?
C2 C3 Re1 72.3(4) . . ?
C4 C3 Re1 71.2(4) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
Re1 C3 H3 128.3 . . ?
C5 C4 C3 121.2(8) . . ?
C5 C4 Re1 73.7(4) . . ?
C3 C4 Re1 72.2(4) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
Re1 C4 H4 126.6 . . ?
C4 C5 C6 119.3(7) . . ?
C4 C5 Re1 71.0(4) . . ?
C6 C5 Re1 71.0(4) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
Re1 C5 H5 130.1 . . ?
C5 C6 C1 120.8(8) . . ?
C5 C6 Re1 73.1(4) . . ?
C1 C6 Re1 72.9(4) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
Re1 C6 H6 126.2 . . ?
O1 C7 C8 114(2) . . ?
O1 C7 C8B 104.8(11) . . ?
O1 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
O1 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
O1 C7 H7C 110.8 . . ?
C8B C7 H7C 110.8 . . ?
O1 C7 H7D 110.8 . . ?
C8B C7 H7D 110.8 . . ?
H7C C7 H7D 108.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8B H8B1 109.5 . . ?
C7 C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7 C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
O2 C9 C10 109.8(9) . . ?
O2 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
O2 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O3 C11 C12 108.3(18) . . ?
O3 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
O3 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O3 C11B C12B 109(2) . . ?
O3 C11B H11C 109.9 . . ?
C12B C11B H11C 109.9 . . ?
O3 C11B H11D 109.9 . . ?
C12B C11B H11D 109.9 . . ?
H11C C11B H11D 108.3 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
O4 C13 C14 108.4(13) . . ?
O4 C13 H13A 110.0 . . ?
C14 C13 H13A 110.0 . . ?
O4 C13 H13B 110.0 . . ?
C14 C13 H13B 110.0 . . ?
H13A C13 H13B 108.4 . . ?
C13 C14 H14C 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14C C14 H14B 109.5 . . ?
C13 C14 H14A 109.5 . . ?
H14C C14 H14A 109.5 . . ?
H14B C14 H14A 109.5 . . ?
O5 C15 C16 118.5(14) . . ?
O5 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
C15 C16 H16C 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16C C16 H16B 109.5 . . ?
C15 C16 H16A 109.5 . . ?
H16C C16 H16A 109.5 . . ?
H16B C16 H16A 109.5 . . ?
C18 C17 O6 108.0(8) . . ?
C18 C17 H17A 110.1 . . ?
O6 C17 H17A 110.1 . . ?
C18 C17 H17B 110.1 . . ?
O6 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O7 C19 C20 100.0(14) . . ?
O7 C19 H19A 111.8 . . ?
C20 C19 H19A 111.8 . . ?
O7 C19 H19B 111.8 . . ?
C20 C19 H19B 111.8 . . ?
H19A C19 H19B 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O7 C19B C20B 111.4(18) . . ?
O7 C19B H19C 109.3 . . ?
C20B C19B H19C 109.3 . . ?
O7 C19B H19D 109.3 . . ?
C20B C19B H19D 109.3 . . ?
H19C C19B H19D 108.0 . . ?
C19B C20B H20D 109.5 . . ?
C19B C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
C19B C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
O8 C21 C22 109.5(7) . . ?
O8 C21 H21A 109.8 . . ?
C22 C21 H21A 109.8 . . ?
O8 C21 H21B 109.8 . . ?
C22 C21 H21B 109.8 . . ?
H21A C21 H21B 108.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 O9 107.7(8) . . ?
C24 C23 H23A 110.2 . . ?
O9 C23 H23A 110.2 . . ?
C24 C23 H23B 110.2 . . ?
O9 C23 H23B 110.2 . . ?
H23A C23 H23B 108.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 O1 P1 128.8(7) . . ?
C9 O2 P1 123.2(5) . . ?
C11B O3 P1 134.7(13) . . ?
C11 O3 P1 126.1(8) . . ?
C13 O4 P2 127.1(8) . . ?
C15 O5 P2 130.5(8) . . ?
C17 O6 P2 122.1(5) . . ?
C19 O7 P3 130.7(7) . . ?
C19B O7 P3 131.4(9) . . ?
C21 O8 P3 122.9(5) . . ?
C23 O9 P3 119.7(5) . . ?
F33 C31 F32 113(2) . . ?
F33 C31 F31 110(3) . . ?
F32 C31 F31 109(2) . . ?
F33 C31 S31 110.4(19) . . ?
F32 C31 S31 109(2) . . ?
F31 C31 S31 106.0(16) . . ?
O32 S31 O33 107(2) . . ?
O32 S31 O31 114.2(9) . . ?
O33 S31 O31 99.5(14) . . ?
O32 S31 C31 107.4(18) . . ?
O33 S31 C31 107.0(15) . . ?
O31 S31 C31 120.6(10) . . ?
O35 S32 O31 127.1(19) . . ?
O35 S32 O34 114(2) . . ?
O31 S32 O34 110.8(10) . . ?
O35 S32 C32 104.7(15) . . ?
O31 S32 C32 96.6(12) . . ?
O34 S32 C32 95.7(15) . . ?
F34 C32 F36 109(2) . . ?
F34 C32 F35 91(2) . . ?
F36 C32 F35 108(2) . . ?
F34 C32 S32 121.8(18) . . ?
F36 C32 S32 106.4(16) . . ?
F35 C32 S32 120.0(15) . . ?
O2 P1 O3 98.2(3) . . ?
O2 P1 O1 102.9(4) . . ?
O3 P1 O1 102.4(4) . . ?
O2 P1 Re1 122.4(3) . . ?
O3 P1 Re1 119.3(2) . . ?
O1 P1 Re1 108.9(2) . . ?
O6 P2 O4 103.1(4) . . ?
O6 P2 O5 97.6(3) . . ?
O4 P2 O5 105.3(4) . . ?
O6 P2 Re1 121.5(2) . . ?
O4 P2 Re1 109.4(3) . . ?
O5 P2 Re1 117.9(2) . . ?
O7 P3 O8 101.6(3) . . ?
O7 P3 O9 99.1(3) . . ?
O8 P3 O9 102.6(3) . . ?
O7 P3 Re1 120.4(2) . . ?
O8 P3 Re1 109.94(18) . . ?
O9 P3 Re1 120.38(19) . . ?

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 C1 C2 C3 1.9(10) . . . . ?
Re1 C1 C2 C3 56.3(6) . . . . ?
C6 C1 C2 Re1 -54.4(6) . . . . ?
C1 C2 C3 C4 -1.1(11) . . . . ?
Re1 C2 C3 C4 55.4(6) . . . . ?
C1 C2 C3 Re1 -56.5(6) . . . . ?
C2 C3 C4 C5 1.5(11) . . . . ?
Re1 C3 C4 C5 57.4(6) . . . . ?
C2 C3 C4 Re1 -55.9(6) . . . . ?
C3 C4 C5 C6 -2.7(10) . . . . ?
Re1 C4 C5 C6 54.0(6) . . . . ?
C3 C4 C5 Re1 -56.7(6) . . . . ?
C4 C5 C6 C1 3.5(10) . . . . ?
Re1 C5 C6 C1 57.5(6) . . . . ?
C4 C5 C6 Re1 -54.0(6) . . . . ?
C2 C1 C6 C5 -3.1(10) . . . . ?
Re1 C1 C6 C5 -57.6(6) . . . . ?
C2 C1 C6 Re1 54.5(6) . . . . ?
C8 C7 O1 P1 -128(4) . . . . ?
C8B C7 O1 P1 176.0(12) . . . . ?
C10 C9 O2 P1 -161.4(9) . . . . ?
C12B C11B O3 P1 150.5(14) . . . . ?
C12 C11 O3 P1 -170.0(15) . . . . ?
C14 C13 O4 P2 144.6(12) . . . . ?
C16 C15 O5 P2 -169.8(12) . . . . ?
C18 C17 O6 P2 -162.5(6) . . . . ?
C20 C19 O7 P3 162.5(19) . . . . ?
C20B C19B O7 P3 -164.8(14) . . . . ?
C22 C21 O8 P3 141.7(6) . . . . ?
C24 C23 O9 P3 -164.5(7) . . . . ?
F33 C31 S31 O32 63(3) . . . . ?
F32 C31 S31 O32 -172(2) . . . . ?
F31 C31 S31 O32 -56(3) . . . . ?
F33 C31 S31 O33 177(3) . . . . ?
F32 C31 S31 O33 -58(2) . . . . ?
F31 C31 S31 O33 58(3) . . . . ?
F33 C31 S31 O31 -70(3) . . . . ?
F32 C31 S31 O31 54(2) . . . . ?
F31 C31 S31 O31 170.7(16) . . . . ?
O35 S32 C32 F34 -63(3) . . . . ?
O31 S32 C32 F34 166(2) . . . . ?
O34 S32 C32 F34 54(2) . . . . ?
O35 S32 C32 F36 63(3) . . . . ?
O31 S32 C32 F36 -67.7(18) . . . . ?
O34 S32 C32 F36 -179.5(18) . . . . ?
O35 S32 C32 F35 -174(3) . . . . ?
O31 S32 C32 F35 54(2) . . . . ?
O34 S32 C32 F35 -57(2) . . . . ?
C9 O2 P1 O3 169.4(8) . . . . ?
C9 O2 P1 O1 -85.8(9) . . . . ?
C9 O2 P1 Re1 36.8(9) . . . . ?
C11B O3 P1 O2 -7(2) . . . . ?
C11 O3 P1 O2 29.4(12) . . . . ?
C11B O3 P1 O1 -113(2) . . . . ?
C11 O3 P1 O1 -75.8(12) . . . . ?
C11B O3 P1 Re1 127(2) . . . . ?
C11 O3 P1 Re1 163.9(11) . . . . ?
C7 O1 P1 O2 -31.6(11) . . . . ?
C7 O1 P1 O3 70.0(11) . . . . ?
C7 O1 P1 Re1 -162.8(10) . . . . ?
C17 O6 P2 O4 -83.3(7) . . . . ?
C17 O6 P2 O5 168.9(6) . . . . ?
C17 O6 P2 Re1 39.5(7) . . . . ?
C13 O4 P2 O6 -35.7(11) . . . . ?
C13 O4 P2 O5 66.1(11) . . . . ?
C13 O4 P2 Re1 -166.3(10) . . . . ?
C15 O5 P2 O6 33.2(14) . . . . ?
C15 O5 P2 O4 -72.7(14) . . . . ?
C15 O5 P2 Re1 165.0(13) . . . . ?
C19 O7 P3 O8 -140.6(11) . . . . ?
C19B O7 P3 O8 -93.1(15) . . . . ?
C19 O7 P3 O9 -35.6(11) . . . . ?
C19B O7 P3 O9 11.9(15) . . . . ?
C19 O7 P3 Re1 97.8(10) . . . . ?
C19B O7 P3 Re1 145.3(15) . . . . ?
C21 O8 P3 O7 54.2(6) . . . . ?
C21 O8 P3 O9 -48.0(6) . . . . ?
C21 O8 P3 Re1 -177.2(5) . . . . ?
C23 O9 P3 O7 -179.1(6) . . . . ?
C23 O9 P3 O8 -74.9(6) . . . . ?
C23 O9 P3 Re1 47.5(6) . . . . ?

_refine_diff_density_max         4.771
_refine_diff_density_min         -2.578
_refine_diff_density_rms         0.134

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_GIM090915
_database_code_depnum_ccdc_archive 'CCDC 1554401'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H53 F3 O12 P3 Re S'
_chemical_formula_weight         961.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4629(3)
_cell_length_b                   12.2103(3)
_cell_length_c                   15.7908(4)
_cell_angle_alpha                97.165(2)
_cell_angle_beta                 102.359(2)
_cell_angle_gamma                94.246(2)
_cell_volume                     1944.62(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    18889
_cell_measurement_theta_min      2.9180
_cell_measurement_theta_max      32.6680

_exptl_crystal_description       bLock
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_F_000             972
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    3.371
_shelx_estimated_absorpt_T_min   0.250
_shelx_estimated_absorpt_T_max   0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.38979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Oxford Xcalibur Ruby CCD'
_diffrn_measurement_method       'ο oscillation scan'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            42674
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.483
_diffrn_reflns_theta_max         33.380
_diffrn_reflns_theta_full        30.44
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13377
_reflns_number_gt                11837
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro (Oxford, 2007)'
_computing_cell_refinement       'CrysAlisPro (Oxford, 2007)'
_computing_data_reduction        'CrysAlisPro (Oxford, 2007)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0327P)²+1.3539P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13377
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0769
_refine_ls_wR_factor_gt          0.0715
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.81409(2) 0.29471(2) 0.80005(2) 0.02341(3) Uani 1 1 d . . . . .
C1 C 0.9698(3) 0.4297(2) 0.87789(19) 0.0349(6) Uani 1 1 d . . . . .
H1A H 0.9756 0.5060 0.8711 0.042 Uiso 1 1 calc R U . . .
C2 C 0.8965(3) 0.3918(3) 0.93578(18) 0.0348(6) Uani 1 1 d . . . . .
H2A H 0.8562 0.4428 0.9696 0.042 Uiso 1 1 calc R U . . .
C3 C 0.8832(3) 0.2783(3) 0.94319(17) 0.0330(6) Uani 1 1 d . . . . .
H3A H 0.8242 0.2512 0.9757 0.040 Uiso 1 1 calc R U . . .
C4 C 0.9586(3) 0.2026(2) 0.90172(17) 0.0303(5) Uani 1 1 d . . . . .
C5 C 0.9602(3) 0.0895(3) 0.9155(2) 0.0383(7) Uani 1 1 d . . . . .
H5A H 0.9063 0.0604 0.9505 0.046 Uiso 1 1 calc R U . . .
C6 C 1.0380(3) 0.0234(3) 0.8790(2) 0.0452(8) Uani 1 1 d . . . . .
H6A H 1.0399 -0.0514 0.8898 0.054 Uiso 1 1 calc R U . . .
C7 C 1.1164(3) 0.0643(3) 0.8250(2) 0.0441(7) Uani 1 1 d . . . . .
H7A H 1.1724 0.0172 0.8015 0.053 Uiso 1 1 calc R U . . .
C8 C 1.1132(3) 0.1692(3) 0.8062(2) 0.0385(7) Uani 1 1 d . . . . .
H8A H 1.1632 0.1937 0.7673 0.046 Uiso 1 1 calc R U . . .
C9 C 1.0350(3) 0.2434(2) 0.84462(18) 0.0306(5) Uani 1 1 d . . . . .
C10 C 1.0340(3) 0.3562(2) 0.83051(19) 0.0316(6) Uani 1 1 d . . . . .
H10A H 1.0773 0.3818 0.7885 0.038 Uiso 1 1 calc R U . . .
C11 C 0.6985(4) 0.6499(3) 0.8245(3) 0.0487(8) Uani 1 1 d . . . . .
H11B H 0.6200 0.6740 0.8441 0.058 Uiso 1 1 calc R U . . .
H11A H 0.6890 0.6603 0.7624 0.058 Uiso 1 1 calc R U . . .
C12 C 0.8212(4) 0.7177(3) 0.8801(4) 0.0704(14) Uani 1 1 d . . . . .
H12C H 0.8980 0.6958 0.8584 0.106 Uiso 1 1 calc R U . . .
H12B H 0.8317 0.7046 0.9411 0.106 Uiso 1 1 calc R U . . .
H12A H 0.8136 0.7967 0.8768 0.106 Uiso 1 1 calc R U . . .
C13 C 0.8517(4) 0.5257(3) 0.6666(2) 0.0452(8) Uani 1 1 d . . . . .
H13B H 0.9070 0.4645 0.6780 0.054 Uiso 1 1 calc R U . . .
H13A H 0.8915 0.5920 0.7096 0.054 Uiso 1 1 calc R U . . .
C14 C 0.8450(5) 0.5507(4) 0.5761(3) 0.0708(13) Uani 1 1 d . . . . .
H14A H 0.8066 0.4845 0.5340 0.106 Uiso 1 1 calc R U . . .
H14B H 0.9339 0.5726 0.5693 0.106 Uiso 1 1 calc R U . . .
H14C H 0.7902 0.6115 0.5654 0.106 Uiso 1 1 calc R U . . .
C15 C 0.4456(3) 0.4803(3) 0.7025(3) 0.0518(9) Uani 1 1 d . . . . .
H15B H 0.4659 0.5227 0.6567 0.062 Uiso 1 1 calc R U . . .
H15A H 0.4491 0.5332 0.7560 0.062 Uiso 1 1 calc R U . . .
C16 C 0.3126(4) 0.4186(3) 0.6720(3) 0.0645(12) Uani 1 1 d . . . . .
H16A H 0.3079 0.3707 0.6166 0.097 Uiso 1 1 calc R U . . .
H16B H 0.2465 0.4714 0.6632 0.097 Uiso 1 1 calc R U . . .
H16C H 0.2955 0.3731 0.7161 0.097 Uiso 1 1 calc R U . . .
C17 C 0.5603(4) 0.0054(3) 0.8691(3) 0.0491(9) Uani 1 1 d . . . . .
H17A H 0.5299 -0.0498 0.8156 0.059 Uiso 1 1 calc R U . . .
H17B H 0.4835 0.0414 0.8818 0.059 Uiso 1 1 calc R U . . .
C18 C 0.6201(4) -0.0505(3) 0.9437(3) 0.0597(11) Uani 1 1 d . . . . .
H18C H 0.6490 0.0045 0.9966 0.090 Uiso 1 1 calc R U . . .
H18B H 0.6960 -0.0861 0.9307 0.090 Uiso 1 1 calc R U . . .
H18A H 0.5550 -0.1068 0.9533 0.090 Uiso 1 1 calc R U . . .
C19 C 0.5406(3) 0.3067(3) 0.92702(19) 0.0394(7) Uani 1 1 d . . . . .
H19A H 0.6051 0.3707 0.9281 0.047 Uiso 1 1 calc R U . . .
H19B H 0.5794 0.2622 0.9724 0.047 Uiso 1 1 calc R U . . .
C20 C 0.4157(4) 0.3468(4) 0.9451(3) 0.0572(10) Uani 1 1 d . . . . .
H20C H 0.3516 0.2830 0.9423 0.086 Uiso 1 1 calc R U . . .
H20B H 0.3799 0.3933 0.9013 0.086 Uiso 1 1 calc R U . . .
H20A H 0.4341 0.3905 1.0037 0.086 Uiso 1 1 calc R U . . .
C21 C 0.3942(3) 0.1019(3) 0.6880(2) 0.0440(8) Uani 1 1 d . . . . .
H21A H 0.3490 0.1689 0.6771 0.053 Uiso 1 1 calc R U . . .
H21B H 0.3667 0.0723 0.7377 0.053 Uiso 1 1 calc R U . . .
C22 C 0.3575(4) 0.0171(3) 0.6087(2) 0.0559(10) Uani 1 1 d . . . . .
H22C H 0.3946 -0.0519 0.6219 0.084 Uiso 1 1 calc R U . . .
H22B H 0.3923 0.0441 0.5613 0.084 Uiso 1 1 calc R U . . .
H22A H 0.2615 0.0031 0.5905 0.084 Uiso 1 1 calc R U . . .
C23 C 0.8134(4) 0.0127(3) 0.6755(2) 0.0435(7) Uani 1 1 d . . . . .
H23A H 0.8176 0.0398 0.7379 0.052 Uiso 1 1 calc R U . . .
H23B H 0.9035 0.0005 0.6690 0.052 Uiso 1 1 calc R U . . .
C24 C 0.7258(4) -0.0940(3) 0.6478(3) 0.0563(10) Uani 1 1 d . . . . .
H24C H 0.7242 -0.1217 0.5865 0.084 Uiso 1 1 calc R U . . .
H24B H 0.6365 -0.0814 0.6537 0.084 Uiso 1 1 calc R U . . .
H24A H 0.7594 -0.1489 0.6849 0.084 Uiso 1 1 calc R U . . .
C25 C 0.5772(3) 0.2455(3) 0.5435(2) 0.0378(7) Uani 1 1 d . . . . .
H25A H 0.5330 0.2607 0.5926 0.045 Uiso 1 1 calc R U . . .
H25B H 0.5540 0.1665 0.5176 0.045 Uiso 1 1 calc R U . . .
C26 C 0.5344(5) 0.3189(3) 0.4758(3) 0.0616(11) Uani 1 1 d . . . . .
H26C H 0.5811 0.3049 0.4285 0.092 Uiso 1 1 calc R U . . .
H26B H 0.5548 0.3968 0.5027 0.092 Uiso 1 1 calc R U . . .
H26A H 0.4395 0.3032 0.4518 0.092 Uiso 1 1 calc R U . . .
C27 C 0.9588(6) 0.2207(6) 0.5414(3) 0.099(2) Uani 1 1 d . . . . .
H27A H 0.8783 0.1755 0.5059 0.119 Uiso 1 1 calc R U . . .
H27B H 0.9671 0.2908 0.5167 0.119 Uiso 1 1 calc R U . . .
C28 C 1.0603(7) 0.1674(7) 0.5348(4) 0.133(3) Uani 1 1 d . . . . .
H28C H 1.1410 0.2137 0.5664 0.199 Uiso 1 1 calc R U . . .
H28B H 1.0626 0.1500 0.4728 0.199 Uiso 1 1 calc R U . . .
H28A H 1.0537 0.0984 0.5600 0.199 Uiso 1 1 calc R U . . .
C30 C 1.1922(6) 0.7542(4) 0.7260(3) 0.0719(14) Uani 1 1 d . . . . .
O1 O 0.7100(2) 0.53389(17) 0.83364(14) 0.0399(5) Uani 1 1 d . . . . .
O2 O 0.7205(2) 0.49442(17) 0.67560(14) 0.0371(5) Uani 1 1 d . . . . .
O3 O 0.5392(2) 0.40190(17) 0.72080(14) 0.0333(4) Uani 1 1 d . . . . .
O4 O 0.6583(2) 0.08791(17) 0.85568(14) 0.0364(5) Uani 1 1 d . . . . .
O5 O 0.5100(2) 0.23979(17) 0.84183(13) 0.0318(4) Uani 1 1 d . . . . .
O6 O 0.5341(2) 0.13009(17) 0.70903(13) 0.0337(4) Uani 1 1 d . . . . .
O7 O 0.7628(2) 0.09349(17) 0.62252(13) 0.0377(5) Uani 1 1 d . . . . .
O8 O 0.7167(2) 0.26865(19) 0.57414(13) 0.0393(5) Uani 1 1 d . . . . .
O9 O 0.9434(2) 0.2468(2) 0.63202(16) 0.0521(7) Uani 1 1 d . . . . .
O10 O 1.3715(4) 0.6920(4) 0.8363(3) 0.1064(15) Uani 1 1 d . . . . .
O11 O 1.2317(4) 0.8142(3) 0.8901(2) 0.0838(11) Uani 1 1 d . . . . .
O12 O 1.1514(5) 0.6252(3) 0.8313(3) 0.1090(15) Uani 1 1 d . . . . .
F1 F 1.2544(5) 0.8435(3) 0.7140(3) 0.1418(19) Uani 1 1 d . . . . .
F2 F 1.1901(5) 0.6713(3) 0.66347(18) 0.1086(13) Uani 1 1 d . . . . .
F3 F 1.0663(5) 0.7838(3) 0.7132(3) 0.1258(15) Uani 1 1 d . . . . .
P1 P 0.69343(7) 0.43335(6) 0.75548(4) 0.02698(13) Uani 1 1 d . . . . .
P2 P 0.62308(7) 0.18808(6) 0.80085(4) 0.02580(13) Uani 1 1 d . . . . .
P3 P 0.80330(7) 0.22356(6) 0.65543(5) 0.03000(15) Uani 1 1 d . . . . .
S1 S 1.24055(9) 0.71678(7) 0.83313(6) 0.04354(18) 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
Re1 C3 2.260(3) . ?
Re1 C1 2.263(3) . ?
Re1 C2 2.273(3) . ?
Re1 P1 2.2778(8) . ?
Re1 C10 2.295(3) . ?
Re1 P2 2.3062(7) . ?
Re1 P3 2.3158(7) . ?
Re1 C4 2.407(3) . ?
Re1 C9 2.420(3) . ?
C1 C10 1.398(4) . ?
C1 C2 1.411(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.404(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.443(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.426(4) . ?
C4 C9 1.435(4) . ?
C5 C6 1.352(5) . ?
C5 H5A 0.9500 . ?
C6 C7 1.412(5) . ?
C6 H6A 0.9500 . ?
C7 C8 1.352(5) . ?
C7 H7A 0.9500 . ?
C8 C9 1.430(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.423(4) . ?
C10 H10A 0.9500 . ?
C11 O1 1.452(4) . ?
C11 C12 1.511(5) . ?
C11 H11B 0.9900 . ?
C11 H11A 0.9900 . ?
C12 H12C 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12A 0.9800 . ?
C13 O2 1.438(4) . ?
C13 C14 1.486(5) . ?
C13 H13B 0.9900 . ?
C13 H13A 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O3 1.430(4) . ?
C15 C16 1.484(5) . ?
C15 H15B 0.9900 . ?
C15 H15A 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 O4 1.451(4) . ?
C17 C18 1.481(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18C 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18A 0.9800 . ?
C19 O5 1.443(3) . ?
C19 C20 1.499(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20C 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20A 0.9800 . ?
C21 O6 1.436(4) . ?
C21 C22 1.482(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22C 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22A 0.9800 . ?
C23 O7 1.431(4) . ?
C23 C24 1.496(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24C 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24A 0.9800 . ?
C25 O8 1.431(4) . ?
C25 C26 1.497(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26C 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26A 0.9800 . ?
C27 C28 1.303(8) . ?
C27 O9 1.471(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28C 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28A 0.9800 . ?
C30 F1 1.284(5) . ?
C30 F2 1.318(6) . ?
C30 F3 1.372(7) . ?
C30 S1 1.785(5) . ?
O1 P1 1.600(2) . ?
O2 P1 1.608(2) . ?
O3 P1 1.590(2) . ?
O4 P2 1.605(2) . ?
O5 P2 1.598(2) . ?
O6 P2 1.593(2) . ?
O7 P3 1.604(2) . ?
O8 P3 1.589(2) . ?
O9 P3 1.601(2) . ?
O10 S1 1.417(4) . ?
O11 S1 1.420(3) . ?
O12 S1 1.396(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Re1 C1 65.15(11) . . ?
C3 Re1 C2 36.09(11) . . ?
C1 Re1 C2 36.26(11) . . ?
C3 Re1 P1 122.00(8) . . ?
C1 Re1 P1 86.87(8) . . ?
C2 Re1 P1 92.52(8) . . ?
C3 Re1 C10 76.54(10) . . ?
C1 Re1 C10 35.70(10) . . ?
C2 Re1 C10 64.59(11) . . ?
P1 Re1 C10 109.54(8) . . ?
C3 Re1 P2 87.62(8) . . ?
C1 Re1 P2 144.84(8) . . ?
C2 Re1 P2 109.15(8) . . ?
P1 Re1 P2 89.73(3) . . ?
C10 Re1 P2 159.56(8) . . ?
C3 Re1 P3 147.80(8) . . ?
C1 Re1 P3 123.28(8) . . ?
C2 Re1 P3 158.99(8) . . ?
P1 Re1 P3 90.17(3) . . ?
C10 Re1 P3 94.90(7) . . ?
P2 Re1 P3 91.69(2) . . ?
C3 Re1 C4 35.86(10) . . ?
C1 Re1 C4 74.90(10) . . ?
C2 Re1 C4 63.69(10) . . ?
P1 Re1 C4 156.15(7) . . ?
C10 Re1 C4 63.26(10) . . ?
P2 Re1 C4 96.35(7) . . ?
P3 Re1 C4 112.59(7) . . ?
C3 Re1 C9 63.70(10) . . ?
C1 Re1 C9 62.98(10) . . ?
C2 Re1 C9 74.51(10) . . ?
P1 Re1 C9 144.49(7) . . ?
C10 Re1 C9 35.00(10) . . ?
P2 Re1 C9 125.66(7) . . ?
P3 Re1 C9 91.39(7) . . ?
C4 Re1 C9 34.60(9) . . ?
C10 C1 C2 120.7(3) . . ?
C10 C1 Re1 73.40(15) . . ?
C2 C1 Re1 72.23(15) . . ?
C10 C1 H1A 119.7 . . ?
C2 C1 H1A 119.7 . . ?
Re1 C1 H1A 126.6 . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 Re1 71.45(15) . . ?
C1 C2 Re1 71.51(15) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
Re1 C2 H2A 129.3 . . ?
C2 C3 C4 120.4(3) . . ?
C2 C3 Re1 72.46(16) . . ?
C4 C3 Re1 77.62(15) . . ?
C2 C3 H3A 119.8 . . ?
C4 C3 H3A 119.8 . . ?
Re1 C3 H3A 121.3 . . ?
C5 C4 C9 119.0(3) . . ?
C5 C4 C3 122.5(3) . . ?
C9 C4 C3 118.5(3) . . ?
C5 C4 Re1 132.4(2) . . ?
C9 C4 Re1 73.22(16) . . ?
C3 C4 Re1 66.52(16) . . ?
C6 C5 C4 120.4(3) . . ?
C6 C5 H5A 119.8 . . ?
C4 C5 H5A 119.8 . . ?
C5 C6 C7 120.7(3) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
C8 C7 C6 121.2(3) . . ?
C8 C7 H7A 119.4 . . ?
C6 C7 H7A 119.4 . . ?
C7 C8 C9 120.4(3) . . ?
C7 C8 H8A 119.8 . . ?
C9 C8 H8A 119.8 . . ?
C10 C9 C8 122.4(3) . . ?
C10 C9 C4 119.4(3) . . ?
C8 C9 C4 118.2(3) . . ?
C10 C9 Re1 67.70(16) . . ?
C8 C9 Re1 134.7(2) . . ?
C4 C9 Re1 72.18(16) . . ?
C1 C10 C9 120.6(3) . . ?
C1 C10 Re1 70.90(16) . . ?
C9 C10 Re1 77.30(16) . . ?
C1 C10 H10A 119.7 . . ?
C9 C10 H10A 119.7 . . ?
Re1 C10 H10A 123.5 . . ?
O1 C11 C12 108.3(3) . . ?
O1 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
O1 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
H11B C11 H11A 108.4 . . ?
C11 C12 H12C 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12C C12 H12B 109.5 . . ?
C11 C12 H12A 109.5 . . ?
H12C C12 H12A 109.5 . . ?
H12B C12 H12A 109.5 . . ?
O2 C13 C14 108.7(3) . . ?
O2 C13 H13B 109.9 . . ?
C14 C13 H13B 109.9 . . ?
O2 C13 H13A 109.9 . . ?
C14 C13 H13A 109.9 . . ?
H13B C13 H13A 108.3 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O3 C15 C16 108.4(3) . . ?
O3 C15 H15B 110.0 . . ?
C16 C15 H15B 110.0 . . ?
O3 C15 H15A 110.0 . . ?
C16 C15 H15A 110.0 . . ?
H15B C15 H15A 108.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C17 C18 108.6(3) . . ?
O4 C17 H17A 110.0 . . ?
C18 C17 H17A 110.0 . . ?
O4 C17 H17B 110.0 . . ?
C18 C17 H17B 110.0 . . ?
H17A C17 H17B 108.3 . . ?
C17 C18 H18C 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18C C18 H18B 109.5 . . ?
C17 C18 H18A 109.5 . . ?
H18C C18 H18A 109.5 . . ?
H18B C18 H18A 109.5 . . ?
O5 C19 C20 108.3(3) . . ?
O5 C19 H19A 110.0 . . ?
C20 C19 H19A 110.0 . . ?
O5 C19 H19B 110.0 . . ?
C20 C19 H19B 110.0 . . ?
H19A C19 H19B 108.4 . . ?
C19 C20 H20C 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20C C20 H20B 109.5 . . ?
C19 C20 H20A 109.5 . . ?
H20C C20 H20A 109.5 . . ?
H20B C20 H20A 109.5 . . ?
O6 C21 C22 109.1(3) . . ?
O6 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
O6 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
C21 C22 H22C 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22C C22 H22B 109.5 . . ?
C21 C22 H22A 109.5 . . ?
H22C C22 H22A 109.5 . . ?
H22B C22 H22A 109.5 . . ?
O7 C23 C24 109.5(3) . . ?
O7 C23 H23A 109.8 . . ?
C24 C23 H23A 109.8 . . ?
O7 C23 H23B 109.8 . . ?
C24 C23 H23B 109.8 . . ?
H23A C23 H23B 108.2 . . ?
C23 C24 H24C 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24C C24 H24B 109.5 . . ?
C23 C24 H24A 109.5 . . ?
H24C C24 H24A 109.5 . . ?
H24B C24 H24A 109.5 . . ?
O8 C25 C26 107.4(3) . . ?
O8 C25 H25A 110.2 . . ?
C26 C25 H25A 110.2 . . ?
O8 C25 H25B 110.2 . . ?
C26 C25 H25B 110.2 . . ?
H25A C25 H25B 108.5 . . ?
C25 C26 H26C 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26C C26 H26B 109.5 . . ?
C25 C26 H26A 109.5 . . ?
H26C C26 H26A 109.5 . . ?
H26B C26 H26A 109.5 . . ?
C28 C27 O9 113.7(6) . . ?
C28 C27 H27A 108.8 . . ?
O9 C27 H27A 108.8 . . ?
C28 C27 H27B 108.8 . . ?
O9 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 H28C 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28C C28 H28B 109.5 . . ?
C27 C28 H28A 109.5 . . ?
H28C C28 H28A 109.5 . . ?
H28B C28 H28A 109.5 . . ?
F1 C30 F2 111.9(5) . . ?
F1 C30 F3 100.7(5) . . ?
F2 C30 F3 105.9(5) . . ?
F1 C30 S1 114.9(4) . . ?
F2 C30 S1 112.7(4) . . ?
F3 C30 S1 109.6(4) . . ?
C11 O1 P1 126.3(2) . . ?
C13 O2 P1 121.9(2) . . ?
C15 O3 P1 124.7(2) . . ?
C17 O4 P2 123.6(2) . . ?
C19 O5 P2 121.02(19) . . ?
C21 O6 P2 126.98(19) . . ?
C23 O7 P3 120.83(19) . . ?
C25 O8 P3 125.56(19) . . ?
C27 O9 P3 120.7(3) . . ?
O3 P1 O1 105.62(12) . . ?
O3 P1 O2 98.28(12) . . ?
O1 P1 O2 102.98(12) . . ?
O3 P1 Re1 116.74(8) . . ?
O1 P1 Re1 110.75(9) . . ?
O2 P1 Re1 120.53(9) . . ?
O6 P2 O5 98.34(11) . . ?
O6 P2 O4 104.84(12) . . ?
O5 P2 O4 102.93(11) . . ?
O6 P2 Re1 117.86(8) . . ?
O5 P2 Re1 121.30(8) . . ?
O4 P2 Re1 109.46(8) . . ?
O8 P3 O9 97.62(13) . . ?
O8 P3 O7 97.86(12) . . ?
O9 P3 O7 104.05(13) . . ?
O8 P3 Re1 123.77(9) . . ?
O9 P3 Re1 110.15(9) . . ?
O7 P3 Re1 119.80(9) . . ?
O12 S1 O10 114.6(3) . . ?
O12 S1 O11 116.6(3) . . ?
O10 S1 O11 113.5(2) . . ?
O12 S1 C30 103.4(3) . . ?
O10 S1 C30 102.3(3) . . ?
O11 S1 C30 104.1(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 C1 C2 C3 -2.7(4) . . . . ?
Re1 C1 C2 C3 54.7(2) . . . . ?
C10 C1 C2 Re1 -57.4(2) . . . . ?
C1 C2 C3 C4 8.7(4) . . . . ?
Re1 C2 C3 C4 63.5(2) . . . . ?
C1 C2 C3 Re1 -54.8(2) . . . . ?
C2 C3 C4 C5 172.6(3) . . . . ?
Re1 C3 C4 C5 -126.5(3) . . . . ?
C2 C3 C4 C9 -7.3(4) . . . . ?
Re1 C3 C4 C9 53.6(2) . . . . ?
C2 C3 C4 Re1 -60.9(2) . . . . ?
C9 C4 C5 C6 3.5(4) . . . . ?
C3 C4 C5 C6 -176.4(3) . . . . ?
Re1 C4 C5 C6 96.9(4) . . . . ?
C4 C5 C6 C7 -1.6(5) . . . . ?
C5 C6 C7 C8 -1.9(5) . . . . ?
C6 C7 C8 C9 3.3(5) . . . . ?
C7 C8 C9 C10 176.6(3) . . . . ?
C7 C8 C9 C4 -1.3(4) . . . . ?
C7 C8 C9 Re1 -93.7(4) . . . . ?
C5 C4 C9 C10 180.0(3) . . . . ?
C3 C4 C9 C10 -0.1(4) . . . . ?
Re1 C4 C9 C10 50.3(2) . . . . ?
C5 C4 C9 C8 -2.1(4) . . . . ?
C3 C4 C9 C8 177.8(3) . . . . ?
Re1 C4 C9 C8 -131.8(3) . . . . ?
C5 C4 C9 Re1 129.7(3) . . . . ?
C3 C4 C9 Re1 -50.4(2) . . . . ?
C2 C1 C10 C9 -4.8(4) . . . . ?
Re1 C1 C10 C9 -61.6(2) . . . . ?
C2 C1 C10 Re1 56.8(2) . . . . ?
C8 C9 C10 C1 -171.7(3) . . . . ?
C4 C9 C10 C1 6.1(4) . . . . ?
Re1 C9 C10 C1 58.5(2) . . . . ?
C8 C9 C10 Re1 129.8(3) . . . . ?
C4 C9 C10 Re1 -52.4(2) . . . . ?
C12 C11 O1 P1 -126.9(3) . . . . ?
C14 C13 O2 P1 164.5(3) . . . . ?
C16 C15 O3 P1 -179.8(3) . . . . ?
C18 C17 O4 P2 -162.0(3) . . . . ?
C20 C19 O5 P2 177.5(2) . . . . ?
C22 C21 O6 P2 -160.7(3) . . . . ?
C24 C23 O7 P3 159.0(2) . . . . ?
C26 C25 O8 P3 170.9(3) . . . . ?
C28 C27 O9 P3 -133.2(6) . . . . ?
C15 O3 P1 O1 46.7(3) . . . . ?
C15 O3 P1 O2 -59.4(3) . . . . ?
C15 O3 P1 Re1 170.2(3) . . . . ?
C11 O1 P1 O3 -80.8(3) . . . . ?
C11 O1 P1 O2 21.8(3) . . . . ?
C11 O1 P1 Re1 152.0(2) . . . . ?
C13 O2 P1 O3 -170.3(2) . . . . ?
C13 O2 P1 O1 81.5(3) . . . . ?
C13 O2 P1 Re1 -42.4(3) . . . . ?
C21 O6 P2 O5 -19.4(3) . . . . ?
C21 O6 P2 O4 86.5(3) . . . . ?
C21 O6 P2 Re1 -151.6(2) . . . . ?
C19 O5 P2 O6 -177.8(2) . . . . ?
C19 O5 P2 O4 74.8(2) . . . . ?
C19 O5 P2 Re1 -47.9(2) . . . . ?
C17 O4 P2 O6 -52.8(3) . . . . ?
C17 O4 P2 O5 49.6(3) . . . . ?
C17 O4 P2 Re1 179.8(2) . . . . ?
C25 O8 P3 O9 162.6(2) . . . . ?
C25 O8 P3 O7 57.2(3) . . . . ?
C25 O8 P3 Re1 -76.9(2) . . . . ?
C27 O9 P3 O8 -42.9(4) . . . . ?
C27 O9 P3 O7 57.2(4) . . . . ?
C27 O9 P3 Re1 -173.2(4) . . . . ?
C23 O7 P3 O8 -178.2(2) . . . . ?
C23 O7 P3 O9 81.8(3) . . . . ?
C23 O7 P3 Re1 -41.7(3) . . . . ?
F1 C30 S1 O12 174.6(5) . . . . ?
F2 C30 S1 O12 -55.5(5) . . . . ?
F3 C30 S1 O12 62.2(4) . . . . ?
F1 C30 S1 O10 -66.0(5) . . . . ?
F2 C30 S1 O10 63.9(5) . . . . ?
F3 C30 S1 O10 -178.5(3) . . . . ?
F1 C30 S1 O11 52.4(5) . . . . ?
F2 C30 S1 O11 -177.8(5) . . . . ?
F3 C30 S1 O11 -60.1(4) . . . . ?

_refine_diff_density_max         1.617
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.132

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_hb130217
_database_code_depnum_ccdc_archive 'CCDC 1554159'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Tc(Me5Ph)(PhBr)]Cl'
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H21 Br Tc, Cl'
_chemical_formula_sum            'C17 H21 Br Cl Tc'
_chemical_formula_weight         438.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.0418(4)
_cell_length_b                   9.2033(5)
_cell_length_c                   12.4028(7)
_cell_angle_alpha                87.599(5)
_cell_angle_beta                 86.191(5)
_cell_angle_gamma                85.980(4)
_cell_volume                     799.48(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    3675
_cell_measurement_theta_min      2.8260
_cell_measurement_theta_max      29.8600

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             436
_exptl_absorpt_coefficient_mu    3.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4953
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.16a (Rigaku Oxford Diffraction, 2015)
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  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 200000
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8837
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         28.28
_reflns_number_total             3914
_reflns_number_gt                3075
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.39.16a (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.16a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16a (Rigaku OD, 2015)'
_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)+(0.0580P)²+0.0678P] 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         3914
_refine_ls_number_parameters     186
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1043
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tc1 Tc 0.39353(5) 0.75070(3) 0.23533(3) 0.01674(11) Uani 1 1 d . . .
Cl3 Cl 0.3755(2) 0.75689(12) -0.20618(10) 0.0408(3) Uani 1 1 d . . .
C13 C 0.5959(6) 0.8829(4) 0.3131(3) 0.0223(9) Uani 1 1 d . . .
H13A H 0.5732 0.9746 0.3456 0.027 Uiso 1 1 calc R . .
C12 C 0.5736(6) 0.7532(4) 0.3754(3) 0.0241(9) Uani 1 1 d . . .
C1 C 0.2076(6) 0.7741(4) 0.0944(3) 0.0242(9) Uani 1 1 d . . .
H1A H 0.2433 0.7866 0.0195 0.029 Uiso 1 1 calc R . .
C17 C 0.6058(6) 0.6159(4) 0.3273(3) 0.0225(9) Uani 1 1 d . . .
H17A H 0.5889 0.5288 0.3696 0.027 Uiso 1 1 calc R . .
C16 C 0.6635(6) 0.6091(4) 0.2159(3) 0.0242(9) Uani 1 1 d . . .
H16A H 0.6870 0.5175 0.1832 0.029 Uiso 1 1 calc R . .
C3 C 0.1146(6) 0.8805(4) 0.2689(3) 0.0250(9) Uani 1 1 d . . .
C14 C 0.6522(6) 0.8758(4) 0.2021(3) 0.0256(9) Uani 1 1 d . . .
H14A H 0.6677 0.9630 0.1595 0.031 Uiso 1 1 calc R . .
C4 C 0.0998(6) 0.7363(5) 0.3172(3) 0.0227(9) Uani 1 1 d . . .
C6 C 0.1955(6) 0.6315(4) 0.1407(3) 0.0236(9) Uani 1 1 d . . .
C2 C 0.1672(6) 0.8984(4) 0.1577(4) 0.0261(9) Uani 1 1 d . . .
C15 C 0.6855(6) 0.7388(5) 0.1540(4) 0.0256(9) Uani 1 1 d . . .
H15A H 0.7232 0.7345 0.0792 0.031 Uiso 1 1 calc R . .
Br1 Br 0.50378(6) 0.76013(5) 0.52575(3) 0.02758(13) Uani 1 1 d . . .
C5 C 0.1412(6) 0.6116(4) 0.2526(3) 0.0237(9) Uani 1 1 d . . .
C10 C 0.1283(7) 0.4585(5) 0.3001(4) 0.0378(12) Uani 1 1 d . . .
H10A H 0.1341 0.4593 0.3787 0.045 Uiso 1 1 calc R . .
H10B H 0.2349 0.3957 0.2696 0.045 Uiso 1 1 calc R . .
H10C H 0.0075 0.4211 0.2826 0.045 Uiso 1 1 calc R . .
C11 C 0.2397(7) 0.5026(5) 0.0691(4) 0.0392(12) Uani 1 1 d . . .
H11A H 0.3360 0.4352 0.1013 0.047 Uiso 1 1 calc R . .
H11B H 0.2885 0.5369 -0.0026 0.047 Uiso 1 1 calc R . .
H11C H 0.1232 0.4523 0.0624 0.047 Uiso 1 1 calc R . .
C8 C 0.0751(7) 1.0128(5) 0.3375(4) 0.0432(13) Uani 1 1 d . . .
H8A H 0.1433 1.0942 0.3041 0.052 Uiso 1 1 calc R . .
H8B H 0.1187 0.9901 0.4100 0.052 Uiso 1 1 calc R . .
H8C H -0.0622 1.0398 0.3426 0.052 Uiso 1 1 calc R . .
C9 C 0.0383(7) 0.7158(6) 0.4351(4) 0.0414(12) Uani 1 1 d . . .
H9A H -0.0299 0.8056 0.4608 0.050 Uiso 1 1 calc R . .
H9B H 0.1509 0.6931 0.4767 0.050 Uiso 1 1 calc R . .
H9C H -0.0462 0.6354 0.4446 0.050 Uiso 1 1 calc R . .
C7 C 0.1795(8) 1.0481(5) 0.1044(4) 0.0446(13) Uani 1 1 d . . .
H7C H 0.0536 1.1007 0.1099 0.054 Uiso 1 1 calc R . .
H7B H 0.2223 1.0388 0.0280 0.054 Uiso 1 1 calc R . .
H7A H 0.2706 1.1019 0.1406 0.054 Uiso 1 1 calc R . .


_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 C17 2.219(4) . ?
Tc1 C12 2.219(4) . ?
Tc1 C15 2.227(4) . ?
Tc1 C13 2.228(4) . ?
Tc1 C14 2.229(4) . ?
Tc1 C16 2.233(4) . ?
Tc1 C1 2.248(4) . ?
Tc1 C3 2.250(4) . ?
Tc1 C6 2.250(4) . ?
Tc1 C4 2.253(4) . ?
Tc1 C5 2.255(4) . ?
Tc1 C2 2.260(4) . ?
C13 C12 1.407(5) . ?
C13 C14 1.410(6) . ?
C12 C17 1.417(5) . ?
C12 Br1 1.899(4) . ?
C1 C6 1.416(5) . ?
C1 C2 1.417(6) . ?
C17 C16 1.418(6) . ?
C16 C15 1.403(6) . ?
C3 C2 1.411(6) . ?
C3 C4 1.441(6) . ?
C3 C8 1.513(6) . ?
C14 C15 1.415(6) . ?
C4 C5 1.429(6) . ?
C4 C9 1.505(6) . ?
C6 C5 1.423(6) . ?
C6 C11 1.514(6) . ?
C2 C7 1.508(6) . ?
C5 C10 1.511(5) . ?

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
C17 Tc1 C12 37.24(14) . . ?
C17 Tc1 C15 66.48(16) . . ?
C12 Tc1 C15 78.45(16) . . ?
C17 Tc1 C13 66.94(14) . . ?
C12 Tc1 C13 36.89(14) . . ?
C15 Tc1 C13 66.62(15) . . ?
C17 Tc1 C14 78.82(15) . . ?
C12 Tc1 C14 66.38(16) . . ?
C15 Tc1 C14 37.05(15) . . ?
C13 Tc1 C14 36.90(15) . . ?
C17 Tc1 C16 37.13(15) . . ?
C12 Tc1 C16 66.81(15) . . ?
C15 Tc1 C16 36.68(15) . . ?
C13 Tc1 C16 78.92(15) . . ?
C14 Tc1 C16 66.59(15) . . ?
C17 Tc1 C1 148.56(15) . . ?
C12 Tc1 C1 173.92(15) . . ?
C15 Tc1 C1 102.28(16) . . ?
C13 Tc1 C1 137.81(14) . . ?
C14 Tc1 C1 110.53(15) . . ?
C16 Tc1 C1 117.34(16) . . ?
C17 Tc1 C3 138.14(15) . . ?
C12 Tc1 C3 110.40(15) . . ?
C15 Tc1 C3 148.38(16) . . ?
C13 Tc1 C3 101.61(15) . . ?
C14 Tc1 C3 116.99(15) . . ?
C16 Tc1 C3 174.63(15) . . ?
C1 Tc1 C3 65.85(15) . . ?
C17 Tc1 C6 117.04(14) . . ?
C12 Tc1 C6 148.79(15) . . ?
C15 Tc1 C6 110.15(16) . . ?
C13 Tc1 C6 173.94(15) . . ?
C14 Tc1 C6 137.74(16) . . ?
C16 Tc1 C6 101.56(15) . . ?
C1 Tc1 C6 36.70(14) . . ?
C3 Tc1 C6 78.49(15) . . ?
C17 Tc1 C4 110.09(15) . . ?
C12 Tc1 C4 101.98(15) . . ?
C15 Tc1 C4 173.80(15) . . ?
C13 Tc1 C4 117.39(15) . . ?
C14 Tc1 C4 148.74(15) . . ?
C16 Tc1 C4 137.77(15) . . ?
C1 Tc1 C4 77.97(15) . . ?
C3 Tc1 C4 37.32(15) . . ?
C6 Tc1 C4 66.31(15) . . ?
C17 Tc1 C5 101.39(14) . . ?
C12 Tc1 C5 117.42(15) . . ?
C15 Tc1 C5 137.43(15) . . ?
C13 Tc1 C5 148.74(15) . . ?
C14 Tc1 C5 173.89(15) . . ?
C16 Tc1 C5 109.88(15) . . ?
C1 Tc1 C5 66.15(15) . . ?
C3 Tc1 C5 66.92(15) . . ?
C6 Tc1 C5 36.82(15) . . ?
C4 Tc1 C5 36.95(15) . . ?
C17 Tc1 C2 174.17(16) . . ?
C12 Tc1 C2 137.73(15) . . ?
C15 Tc1 C2 117.52(16) . . ?
C13 Tc1 C2 110.13(15) . . ?
C14 Tc1 C2 101.88(15) . . ?
C16 Tc1 C2 148.42(16) . . ?
C1 Tc1 C2 36.65(15) . . ?
C3 Tc1 C2 36.45(15) . . ?
C6 Tc1 C2 66.34(15) . . ?
C4 Tc1 C2 66.34(15) . . ?
C5 Tc1 C2 78.54(15) . . ?
C12 C13 C14 119.6(4) . . ?
C12 C13 Tc1 71.2(2) . . ?
C14 C13 Tc1 71.6(2) . . ?
C13 C12 C17 120.6(4) . . ?
C13 C12 Br1 120.2(3) . . ?
C17 C12 Br1 119.2(3) . . ?
C13 C12 Tc1 71.9(2) . . ?
C17 C12 Tc1 71.4(2) . . ?
Br1 C12 Tc1 130.4(2) . . ?
C6 C1 C2 121.1(4) . . ?
C6 C1 Tc1 71.8(2) . . ?
C2 C1 Tc1 72.1(2) . . ?
C12 C17 C16 119.7(4) . . ?
C12 C17 Tc1 71.4(2) . . ?
C16 C17 Tc1 72.0(2) . . ?
C15 C16 C17 119.5(4) . . ?
C15 C16 Tc1 71.4(2) . . ?
C17 C16 Tc1 70.9(2) . . ?
C2 C3 C4 119.9(4) . . ?
C2 C3 C8 119.9(4) . . ?
C4 C3 C8 120.2(4) . . ?
C2 C3 Tc1 72.1(2) . . ?
C4 C3 Tc1 71.4(2) . . ?
C8 C3 Tc1 128.3(3) . . ?
C13 C14 C15 119.9(4) . . ?
C13 C14 Tc1 71.5(2) . . ?
C15 C14 Tc1 71.4(2) . . ?
C5 C4 C3 119.9(4) . . ?
C5 C4 C9 119.6(4) . . ?
C3 C4 C9 120.4(4) . . ?
C5 C4 Tc1 71.6(2) . . ?
C3 C4 Tc1 71.2(2) . . ?
C9 C4 Tc1 130.3(3) . . ?
C1 C6 C5 119.9(4) . . ?
C1 C6 C11 118.9(4) . . ?
C5 C6 C11 121.2(4) . . ?
C1 C6 Tc1 71.5(2) . . ?
C5 C6 Tc1 71.8(2) . . ?
C11 C6 Tc1 129.3(3) . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 C7 121.2(4) . . ?
C1 C2 C7 119.2(4) . . ?
C3 C2 Tc1 71.4(2) . . ?
C1 C2 Tc1 71.2(2) . . ?
C7 C2 Tc1 130.1(3) . . ?
C16 C15 C14 120.7(4) . . ?
C16 C15 Tc1 71.9(2) . . ?
C14 C15 Tc1 71.6(2) . . ?
C6 C5 C4 119.4(4) . . ?
C6 C5 C10 118.9(4) . . ?
C4 C5 C10 121.7(4) . . ?
C6 C5 Tc1 71.4(2) . . ?
C4 C5 Tc1 71.4(2) . . ?
C10 C5 Tc1 129.4(3) . . ?

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
C17 Tc1 C13 C12 -29.0(2) . . . . ?
C15 Tc1 C13 C12 -102.3(3) . . . . ?
C14 Tc1 C13 C12 -131.5(4) . . . . ?
C16 Tc1 C13 C12 -66.0(3) . . . . ?
C1 Tc1 C13 C12 175.3(2) . . . . ?
C3 Tc1 C13 C12 108.6(3) . . . . ?
C6 Tc1 C13 C12 -161.1(13) . . . . ?
C4 Tc1 C13 C12 72.5(3) . . . . ?
C5 Tc1 C13 C12 44.2(4) . . . . ?
C2 Tc1 C13 C12 145.5(2) . . . . ?
C17 Tc1 C13 C14 102.5(3) . . . . ?
C12 Tc1 C13 C14 131.5(4) . . . . ?
C15 Tc1 C13 C14 29.3(2) . . . . ?
C16 Tc1 C13 C14 65.6(2) . . . . ?
C1 Tc1 C13 C14 -53.2(3) . . . . ?
C3 Tc1 C13 C14 -119.9(3) . . . . ?
C6 Tc1 C13 C14 -29.6(15) . . . . ?
C4 Tc1 C13 C14 -156.0(2) . . . . ?
C5 Tc1 C13 C14 175.8(3) . . . . ?
C2 Tc1 C13 C14 -82.9(3) . . . . ?
C14 C13 C12 C17 -0.5(6) . . . . ?
Tc1 C13 C12 C17 54.3(4) . . . . ?
C14 C13 C12 Br1 178.5(3) . . . . ?
Tc1 C13 C12 Br1 -126.7(3) . . . . ?
C14 C13 C12 Tc1 -54.8(3) . . . . ?
C17 Tc1 C12 C13 132.4(4) . . . . ?
C15 Tc1 C12 C13 66.3(3) . . . . ?
C14 Tc1 C12 C13 29.4(2) . . . . ?
C16 Tc1 C12 C13 102.9(3) . . . . ?
C1 Tc1 C12 C13 -31.2(15) . . . . ?
C3 Tc1 C12 C13 -82.1(3) . . . . ?
C6 Tc1 C12 C13 176.2(3) . . . . ?
C4 Tc1 C12 C13 -120.0(3) . . . . ?
C5 Tc1 C12 C13 -155.9(2) . . . . ?
C2 Tc1 C12 C13 -52.2(3) . . . . ?
C15 Tc1 C12 C17 -66.2(2) . . . . ?
C13 Tc1 C12 C17 -132.4(4) . . . . ?
C14 Tc1 C12 C17 -103.0(3) . . . . ?
C16 Tc1 C12 C17 -29.6(2) . . . . ?
C1 Tc1 C12 C17 -163.6(13) . . . . ?
C3 Tc1 C12 C17 145.5(2) . . . . ?
C6 Tc1 C12 C17 43.8(4) . . . . ?
C4 Tc1 C12 C17 107.5(3) . . . . ?
C5 Tc1 C12 C17 71.6(3) . . . . ?
C2 Tc1 C12 C17 175.4(2) . . . . ?
C17 Tc1 C12 Br1 -112.9(4) . . . . ?
C15 Tc1 C12 Br1 -179.0(3) . . . . ?
C13 Tc1 C12 Br1 114.7(4) . . . . ?
C14 Tc1 C12 Br1 144.1(3) . . . . ?
C16 Tc1 C12 Br1 -142.5(3) . . . . ?
C1 Tc1 C12 Br1 83.5(15) . . . . ?
C3 Tc1 C12 Br1 32.6(3) . . . . ?
C6 Tc1 C12 Br1 -69.1(4) . . . . ?
C4 Tc1 C12 Br1 -5.4(3) . . . . ?
C5 Tc1 C12 Br1 -41.2(3) . . . . ?
C2 Tc1 C12 Br1 62.5(4) . . . . ?
C17 Tc1 C1 C6 42.6(4) . . . . ?
C12 Tc1 C1 C6 -156.5(14) . . . . ?
C15 Tc1 C1 C6 107.3(2) . . . . ?
C13 Tc1 C1 C6 175.9(2) . . . . ?
C14 Tc1 C1 C6 145.1(2) . . . . ?
C16 Tc1 C1 C6 71.6(3) . . . . ?
C3 Tc1 C1 C6 -103.6(3) . . . . ?
C4 Tc1 C1 C6 -66.3(3) . . . . ?
C5 Tc1 C1 C6 -29.4(2) . . . . ?
C2 Tc1 C1 C6 -132.7(4) . . . . ?
C17 Tc1 C1 C2 175.3(3) . . . . ?
C12 Tc1 C1 C2 -23.8(15) . . . . ?
C15 Tc1 C1 C2 -120.0(3) . . . . ?
C13 Tc1 C1 C2 -51.4(3) . . . . ?
C14 Tc1 C1 C2 -82.2(3) . . . . ?
C16 Tc1 C1 C2 -155.7(2) . . . . ?
C3 Tc1 C1 C2 29.1(2) . . . . ?
C6 Tc1 C1 C2 132.7(4) . . . . ?
C4 Tc1 C1 C2 66.4(3) . . . . ?
C5 Tc1 C1 C2 103.3(3) . . . . ?
C13 C12 C17 C16 0.8(6) . . . . ?
Br1 C12 C17 C16 -178.1(3) . . . . ?
Tc1 C12 C17 C16 55.4(3) . . . . ?
C13 C12 C17 Tc1 -54.6(4) . . . . ?
Br1 C12 C17 Tc1 126.5(3) . . . . ?
C15 Tc1 C17 C12 102.2(3) . . . . ?
C13 Tc1 C17 C12 28.8(2) . . . . ?
C14 Tc1 C17 C12 65.5(3) . . . . ?
C16 Tc1 C17 C12 131.3(4) . . . . ?
C1 Tc1 C17 C12 176.7(3) . . . . ?
C3 Tc1 C17 C12 -52.7(3) . . . . ?
C6 Tc1 C17 C12 -156.3(2) . . . . ?
C4 Tc1 C17 C12 -83.3(3) . . . . ?
C5 Tc1 C17 C12 -120.7(3) . . . . ?
C2 Tc1 C17 C12 -32.0(15) . . . . ?
C12 Tc1 C17 C16 -131.3(4) . . . . ?
C15 Tc1 C17 C16 -29.0(2) . . . . ?
C13 Tc1 C17 C16 -102.5(3) . . . . ?
C14 Tc1 C17 C16 -65.8(2) . . . . ?
C1 Tc1 C17 C16 45.4(4) . . . . ?
C3 Tc1 C17 C16 176.0(2) . . . . ?
C6 Tc1 C17 C16 72.5(3) . . . . ?
C4 Tc1 C17 C16 145.4(2) . . . . ?
C5 Tc1 C17 C16 108.0(2) . . . . ?
C2 Tc1 C17 C16 -163.3(14) . . . . ?
C12 C17 C16 C15 -0.8(6) . . . . ?
Tc1 C17 C16 C15 54.3(4) . . . . ?
C12 C17 C16 Tc1 -55.1(3) . . . . ?
C17 Tc1 C16 C15 -131.8(4) . . . . ?
C12 Tc1 C16 C15 -102.2(3) . . . . ?
C13 Tc1 C16 C15 -65.5(3) . . . . ?
C14 Tc1 C16 C15 -29.0(3) . . . . ?
C1 Tc1 C16 C15 72.9(3) . . . . ?
C3 Tc1 C16 C15 -161.7(15) . . . . ?
C6 Tc1 C16 C15 108.3(3) . . . . ?
C4 Tc1 C16 C15 175.7(2) . . . . ?
C5 Tc1 C16 C15 145.6(3) . . . . ?
C2 Tc1 C16 C15 45.0(4) . . . . ?
C12 Tc1 C16 C17 29.7(2) . . . . ?
C15 Tc1 C16 C17 131.8(4) . . . . ?
C13 Tc1 C16 C17 66.3(2) . . . . ?
C14 Tc1 C16 C17 102.8(3) . . . . ?
C1 Tc1 C16 C17 -155.3(2) . . . . ?
C3 Tc1 C16 C17 -29.9(17) . . . . ?
C6 Tc1 C16 C17 -119.9(2) . . . . ?
C4 Tc1 C16 C17 -52.5(3) . . . . ?
C5 Tc1 C16 C17 -82.5(3) . . . . ?
C2 Tc1 C16 C17 176.8(3) . . . . ?
C17 Tc1 C3 C2 176.5(2) . . . . ?
C12 Tc1 C3 C2 145.6(2) . . . . ?
C15 Tc1 C3 C2 44.3(4) . . . . ?
C13 Tc1 C3 C2 108.3(3) . . . . ?
C14 Tc1 C3 C2 72.5(3) . . . . ?
C16 Tc1 C3 C2 -156.7(15) . . . . ?
C1 Tc1 C3 C2 -29.2(2) . . . . ?
C6 Tc1 C3 C2 -65.6(2) . . . . ?
C4 Tc1 C3 C2 -131.4(4) . . . . ?
C5 Tc1 C3 C2 -102.3(3) . . . . ?
C17 Tc1 C3 C4 -52.1(3) . . . . ?
C12 Tc1 C3 C4 -83.0(3) . . . . ?
C15 Tc1 C3 C4 175.7(3) . . . . ?
C13 Tc1 C3 C4 -120.3(2) . . . . ?
C14 Tc1 C3 C4 -156.1(2) . . . . ?
C16 Tc1 C3 C4 -25.2(17) . . . . ?
C1 Tc1 C3 C4 102.2(3) . . . . ?
C6 Tc1 C3 C4 65.8(2) . . . . ?
C5 Tc1 C3 C4 29.1(2) . . . . ?
C2 Tc1 C3 C4 131.4(4) . . . . ?
C17 Tc1 C3 C8 62.2(5) . . . . ?
C12 Tc1 C3 C8 31.2(5) . . . . ?
C15 Tc1 C3 C8 -70.1(5) . . . . ?
C13 Tc1 C3 C8 -6.1(5) . . . . ?
C14 Tc1 C3 C8 -41.9(5) . . . . ?
C16 Tc1 C3 C8 89.0(16) . . . . ?
C1 Tc1 C3 C8 -143.6(5) . . . . ?
C6 Tc1 C3 C8 -179.9(5) . . . . ?
C4 Tc1 C3 C8 114.2(5) . . . . ?
C5 Tc1 C3 C8 143.3(5) . . . . ?
C2 Tc1 C3 C8 -114.4(5) . . . . ?
C12 C13 C14 C15 0.1(6) . . . . ?
Tc1 C13 C14 C15 -54.5(4) . . . . ?
C12 C13 C14 Tc1 54.6(4) . . . . ?
C17 Tc1 C14 C13 -66.3(2) . . . . ?
C12 Tc1 C14 C13 -29.4(2) . . . . ?
C15 Tc1 C14 C13 -131.9(4) . . . . ?
C16 Tc1 C14 C13 -103.2(3) . . . . ?
C1 Tc1 C14 C13 145.0(2) . . . . ?
C3 Tc1 C14 C13 72.4(3) . . . . ?
C6 Tc1 C14 C13 175.6(2) . . . . ?
C4 Tc1 C14 C13 44.1(4) . . . . ?
C5 Tc1 C14 C13 -158.9(13) . . . . ?
C2 Tc1 C14 C13 107.8(3) . . . . ?
C17 Tc1 C14 C15 65.6(3) . . . . ?
C12 Tc1 C14 C15 102.5(3) . . . . ?
C13 Tc1 C14 C15 131.9(4) . . . . ?
C16 Tc1 C14 C15 28.7(3) . . . . ?
C1 Tc1 C14 C15 -83.1(3) . . . . ?
C3 Tc1 C14 C15 -155.7(3) . . . . ?
C6 Tc1 C14 C15 -52.6(3) . . . . ?
C4 Tc1 C14 C15 176.0(3) . . . . ?
C5 Tc1 C14 C15 -27.0(15) . . . . ?
C2 Tc1 C14 C15 -120.3(3) . . . . ?
C2 C3 C4 C5 0.9(6) . . . . ?
C8 C3 C4 C5 -178.7(4) . . . . ?
Tc1 C3 C4 C5 -54.6(3) . . . . ?
C2 C3 C4 C9 -178.2(4) . . . . ?
C8 C3 C4 C9 2.2(6) . . . . ?
Tc1 C3 C4 C9 126.3(4) . . . . ?
C2 C3 C4 Tc1 55.5(3) . . . . ?
C8 C3 C4 Tc1 -124.1(4) . . . . ?
C17 Tc1 C4 C5 -82.2(2) . . . . ?
C12 Tc1 C4 C5 -120.1(2) . . . . ?
C15 Tc1 C4 C5 -26.8(15) . . . . ?
C13 Tc1 C4 C5 -155.9(2) . . . . ?
C14 Tc1 C4 C5 176.0(3) . . . . ?
C16 Tc1 C4 C5 -51.5(3) . . . . ?
C1 Tc1 C4 C5 66.2(2) . . . . ?
C3 Tc1 C4 C5 131.9(3) . . . . ?
C6 Tc1 C4 C5 29.4(2) . . . . ?
C2 Tc1 C4 C5 102.8(3) . . . . ?
C17 Tc1 C4 C3 145.9(2) . . . . ?
C12 Tc1 C4 C3 108.0(2) . . . . ?
C15 Tc1 C4 C3 -158.7(13) . . . . ?
C13 Tc1 C4 C3 72.2(3) . . . . ?
C14 Tc1 C4 C3 44.1(4) . . . . ?
C16 Tc1 C4 C3 176.6(2) . . . . ?
C1 Tc1 C4 C3 -65.8(2) . . . . ?
C6 Tc1 C4 C3 -102.5(3) . . . . ?
C5 Tc1 C4 C3 -131.9(3) . . . . ?
C2 Tc1 C4 C3 -29.1(2) . . . . ?
C17 Tc1 C4 C9 31.5(5) . . . . ?
C12 Tc1 C4 C9 -6.4(4) . . . . ?
C15 Tc1 C4 C9 86.9(15) . . . . ?
C13 Tc1 C4 C9 -42.2(5) . . . . ?
C14 Tc1 C4 C9 -70.3(5) . . . . ?
C16 Tc1 C4 C9 62.2(5) . . . . ?
C1 Tc1 C4 C9 179.8(4) . . . . ?
C3 Tc1 C4 C9 -114.4(5) . . . . ?
C6 Tc1 C4 C9 143.1(5) . . . . ?
C5 Tc1 C4 C9 113.7(5) . . . . ?
C2 Tc1 C4 C9 -143.5(5) . . . . ?
C2 C1 C6 C5 0.3(6) . . . . ?
Tc1 C1 C6 C5 55.1(3) . . . . ?
C2 C1 C6 C11 179.8(4) . . . . ?
Tc1 C1 C6 C11 -125.4(4) . . . . ?
C2 C1 C6 Tc1 -54.8(4) . . . . ?
C17 Tc1 C6 C1 -156.6(2) . . . . ?
C12 Tc1 C6 C1 175.3(3) . . . . ?
C15 Tc1 C6 C1 -83.5(3) . . . . ?
C13 Tc1 C6 C1 -26.7(15) . . . . ?
C14 Tc1 C6 C1 -52.9(3) . . . . ?
C16 Tc1 C6 C1 -120.7(3) . . . . ?
C3 Tc1 C6 C1 64.8(3) . . . . ?
C4 Tc1 C6 C1 102.0(3) . . . . ?
C5 Tc1 C6 C1 131.5(4) . . . . ?
C2 Tc1 C6 C1 28.6(2) . . . . ?
C17 Tc1 C6 C5 71.8(3) . . . . ?
C12 Tc1 C6 C5 43.8(4) . . . . ?
C15 Tc1 C6 C5 145.0(2) . . . . ?
C13 Tc1 C6 C5 -158.3(13) . . . . ?
C14 Tc1 C6 C5 175.6(2) . . . . ?
C16 Tc1 C6 C5 107.8(2) . . . . ?
C1 Tc1 C6 C5 -131.5(4) . . . . ?
C3 Tc1 C6 C5 -66.7(2) . . . . ?
C4 Tc1 C6 C5 -29.5(2) . . . . ?
C2 Tc1 C6 C5 -102.9(3) . . . . ?
C17 Tc1 C6 C11 -44.0(4) . . . . ?
C12 Tc1 C6 C11 -72.1(5) . . . . ?
C15 Tc1 C6 C11 29.1(4) . . . . ?
C13 Tc1 C6 C11 85.9(14) . . . . ?
C14 Tc1 C6 C11 59.7(5) . . . . ?
C16 Tc1 C6 C11 -8.0(4) . . . . ?
C1 Tc1 C6 C11 112.6(5) . . . . ?
C3 Tc1 C6 C11 177.4(4) . . . . ?
C4 Tc1 C6 C11 -145.4(4) . . . . ?
C5 Tc1 C6 C11 -115.9(5) . . . . ?
C2 Tc1 C6 C11 141.2(4) . . . . ?
C4 C3 C2 C1 -0.8(6) . . . . ?
C8 C3 C2 C1 178.8(4) . . . . ?
Tc1 C3 C2 C1 54.4(4) . . . . ?
C4 C3 C2 C7 178.6(4) . . . . ?
C8 C3 C2 C7 -1.8(6) . . . . ?
Tc1 C3 C2 C7 -126.3(4) . . . . ?
C4 C3 C2 Tc1 -55.1(3) . . . . ?
C8 C3 C2 Tc1 124.4(4) . . . . ?
C6 C1 C2 C3 0.2(6) . . . . ?
Tc1 C1 C2 C3 -54.5(4) . . . . ?
C6 C1 C2 C7 -179.2(4) . . . . ?
Tc1 C1 C2 C7 126.2(4) . . . . ?
C6 C1 C2 Tc1 54.6(4) . . . . ?
C17 Tc1 C2 C3 -23.4(15) . . . . ?
C12 Tc1 C2 C3 -51.9(3) . . . . ?
C15 Tc1 C2 C3 -155.6(2) . . . . ?
C13 Tc1 C2 C3 -82.2(3) . . . . ?
C14 Tc1 C2 C3 -119.7(2) . . . . ?
C16 Tc1 C2 C3 175.9(3) . . . . ?
C1 Tc1 C2 C3 131.8(4) . . . . ?
C6 Tc1 C2 C3 103.1(3) . . . . ?
C4 Tc1 C2 C3 29.8(2) . . . . ?
C5 Tc1 C2 C3 66.5(3) . . . . ?
C17 Tc1 C2 C1 -155.1(14) . . . . ?
C12 Tc1 C2 C1 176.4(2) . . . . ?
C15 Tc1 C2 C1 72.6(3) . . . . ?
C13 Tc1 C2 C1 146.0(2) . . . . ?
C14 Tc1 C2 C1 108.5(3) . . . . ?
C16 Tc1 C2 C1 44.2(4) . . . . ?
C3 Tc1 C2 C1 -131.8(4) . . . . ?
C6 Tc1 C2 C1 -28.7(2) . . . . ?
C4 Tc1 C2 C1 -102.0(3) . . . . ?
C5 Tc1 C2 C1 -65.3(3) . . . . ?
C17 Tc1 C2 C7 92.1(15) . . . . ?
C12 Tc1 C2 C7 63.6(5) . . . . ?
C15 Tc1 C2 C7 -40.1(5) . . . . ?
C13 Tc1 C2 C7 33.3(5) . . . . ?
C14 Tc1 C2 C7 -4.2(5) . . . . ?
C16 Tc1 C2 C7 -68.6(5) . . . . ?
C1 Tc1 C2 C7 -112.8(5) . . . . ?
C3 Tc1 C2 C7 115.5(5) . . . . ?
C6 Tc1 C2 C7 -141.4(5) . . . . ?
C4 Tc1 C2 C7 145.3(5) . . . . ?
C5 Tc1 C2 C7 -178.0(5) . . . . ?
C17 C16 C15 C14 0.5(6) . . . . ?
Tc1 C16 C15 C14 54.5(4) . . . . ?
C17 C16 C15 Tc1 -54.0(3) . . . . ?
C13 C14 C15 C16 -0.1(6) . . . . ?
Tc1 C14 C15 C16 -54.7(4) . . . . ?
C13 C14 C15 Tc1 54.6(4) . . . . ?
C17 Tc1 C15 C16 29.4(2) . . . . ?
C12 Tc1 C15 C16 66.5(3) . . . . ?
C13 Tc1 C15 C16 103.3(3) . . . . ?
C14 Tc1 C15 C16 132.4(4) . . . . ?
C1 Tc1 C15 C16 -119.7(3) . . . . ?
C3 Tc1 C15 C16 176.8(3) . . . . ?
C6 Tc1 C15 C16 -82.2(3) . . . . ?
C4 Tc1 C15 C16 -28.1(15) . . . . ?
C5 Tc1 C15 C16 -51.7(4) . . . . ?
C2 Tc1 C15 C16 -155.3(2) . . . . ?
C17 Tc1 C15 C14 -103.0(3) . . . . ?
C12 Tc1 C15 C14 -65.9(3) . . . . ?
C13 Tc1 C15 C14 -29.1(2) . . . . ?
C16 Tc1 C15 C14 -132.4(4) . . . . ?
C1 Tc1 C15 C14 107.9(3) . . . . ?
C3 Tc1 C15 C14 44.4(4) . . . . ?
C6 Tc1 C15 C14 145.3(3) . . . . ?
C4 Tc1 C15 C14 -160.5(13) . . . . ?
C5 Tc1 C15 C14 175.9(2) . . . . ?
C2 Tc1 C15 C14 72.3(3) . . . . ?
C1 C6 C5 C4 -0.2(6) . . . . ?
C11 C6 C5 C4 -179.7(4) . . . . ?
Tc1 C6 C5 C4 54.8(3) . . . . ?
C1 C6 C5 C10 179.7(4) . . . . ?
C11 C6 C5 C10 0.1(6) . . . . ?
Tc1 C6 C5 C10 -125.4(4) . . . . ?
C1 C6 C5 Tc1 -55.0(3) . . . . ?
C11 C6 C5 Tc1 125.5(4) . . . . ?
C3 C4 C5 C6 -0.4(6) . . . . ?
C9 C4 C5 C6 178.7(4) . . . . ?
Tc1 C4 C5 C6 -54.8(3) . . . . ?
C3 C4 C5 C10 179.8(4) . . . . ?
C9 C4 C5 C10 -1.1(6) . . . . ?
Tc1 C4 C5 C10 125.4(4) . . . . ?
C3 C4 C5 Tc1 54.4(3) . . . . ?
C9 C4 C5 Tc1 -126.5(4) . . . . ?
C17 Tc1 C5 C6 -120.3(2) . . . . ?
C12 Tc1 C5 C6 -156.2(2) . . . . ?
C15 Tc1 C5 C6 -52.8(3) . . . . ?
C13 Tc1 C5 C6 175.7(3) . . . . ?
C14 Tc1 C5 C6 -28.9(15) . . . . ?
C16 Tc1 C5 C6 -82.7(3) . . . . ?
C1 Tc1 C5 C6 29.3(2) . . . . ?
C3 Tc1 C5 C6 102.0(3) . . . . ?
C4 Tc1 C5 C6 131.3(3) . . . . ?
C2 Tc1 C5 C6 65.6(2) . . . . ?
C17 Tc1 C5 C4 108.4(2) . . . . ?
C12 Tc1 C5 C4 72.5(3) . . . . ?
C15 Tc1 C5 C4 175.9(2) . . . . ?
C13 Tc1 C5 C4 44.4(4) . . . . ?
C14 Tc1 C5 C4 -160.2(13) . . . . ?
C16 Tc1 C5 C4 146.0(2) . . . . ?
C1 Tc1 C5 C4 -102.0(3) . . . . ?
C3 Tc1 C5 C4 -29.4(2) . . . . ?
C6 Tc1 C5 C4 -131.3(3) . . . . ?
C2 Tc1 C5 C4 -65.7(2) . . . . ?
C17 Tc1 C5 C10 -7.8(4) . . . . ?
C12 Tc1 C5 C10 -43.6(4) . . . . ?
C15 Tc1 C5 C10 59.7(5) . . . . ?
C13 Tc1 C5 C10 -71.8(5) . . . . ?
C14 Tc1 C5 C10 83.6(15) . . . . ?
C16 Tc1 C5 C10 29.8(4) . . . . ?
C1 Tc1 C5 C10 141.8(4) . . . . ?
C3 Tc1 C5 C10 -145.5(4) . . . . ?
C6 Tc1 C5 C10 112.5(5) . . . . ?
C4 Tc1 C5 C10 -116.1(5) . . . . ?
C2 Tc1 C5 C10 178.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.495
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.143
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_GIM180516
_database_code_depnum_ccdc_archive 'CCDC 1554400'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H14 F6 Li O6 Re S2'
_chemical_formula_weight         697.55

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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   9.0801(3)
_cell_length_b                   10.7870(3)
_cell_length_c                   11.5849(3)
_cell_angle_alpha                104.912(2)
_cell_angle_beta                 98.624(2)
_cell_angle_gamma                91.639(2)
_cell_volume                     1081.41(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    15556
_cell_measurement_theta_min      2.6760
_cell_measurement_theta_max      34.0310

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_F_000             668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    5.897
_shelx_estimated_absorpt_T_min   0.225
_shelx_estimated_absorpt_T_max   0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.41615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Oxford Xcalibur Ruby CCD'
_diffrn_measurement_method       'ο oscillation scan'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            34421
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.274
_diffrn_reflns_theta_max         35.022
_diffrn_reflns_theta_full        33.07
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             17403
_reflns_number_gt                15889
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_max     0.883
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro (Oxford, 2007)'
_computing_cell_refinement       'CrysAlisPro (Oxford, 2007)'
_computing_data_reduction        'CrysAlisPro (Oxford, 2007)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0304P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_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 x determined using 6880 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         17403
_refine_ls_number_parameters     613
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.07311(2) 0.06112(2) -0.21490(2) 0.02229(7) Uani 1 1 d . . . . .
Re2 Re -0.46488(2) 0.51429(2) -0.24241(2) 0.02207(6) Uani 1 1 d . . . . .
C1 C 0.1633(10) -0.1242(8) -0.3209(8) 0.0262(16) Uani 1 1 d . . . . .
C2 C 0.0324(9) -0.1520(7) -0.2761(8) 0.0327(17) Uani 1 1 d . . . . .
H2A H -0.0516 -0.1975 -0.3312 0.039 Uiso 1 1 calc R U . . .
C3 C 0.0245(11) -0.1141(10) -0.1536(11) 0.043(2) Uani 1 1 d . . . . .
H3A H -0.0621 -0.1379 -0.1251 0.052 Uiso 1 1 calc R U . . .
C4 C 0.1468(14) -0.0392(9) -0.0697(10) 0.039(2) Uani 1 1 d . . . . .
H4A H 0.1422 -0.0150 0.0144 0.047 Uiso 1 1 calc R U . . .
C5 C 0.2709(10) -0.0024(8) -0.1113(8) 0.0351(18) Uani 1 1 d . . . . .
H5A H 0.3483 0.0528 -0.0560 0.042 Uiso 1 1 calc R U . . .
C6 C 0.2852(9) -0.0460(7) -0.2369(7) 0.0260(14) Uani 1 1 d . . . . .
C7 C 0.4129(8) -0.0112(7) -0.2838(8) 0.0364(17) Uani 1 1 d . . . . .
H7A H 0.4939 0.0409 -0.2301 0.044 Uiso 1 1 calc R U . . .
C8 C 0.4200(9) -0.0511(8) -0.4032(9) 0.0390(18) Uani 1 1 d . . . . .
H8A H 0.5061 -0.0270 -0.4320 0.047 Uiso 1 1 calc R U . . .
C9 C 0.3012(10) -0.1284(8) -0.4859(8) 0.0387(18) Uani 1 1 d . . . . .
H9A H 0.3091 -0.1561 -0.5694 0.046 Uiso 1 1 calc R U . . .
C10 C 0.1771(9) -0.1630(7) -0.4477(7) 0.0350(15) Uani 1 1 d . . . . .
H10A H 0.0977 -0.2135 -0.5047 0.042 Uiso 1 1 calc R U . . .
C11 C 0.0026(14) 0.1531(12) -0.3625(11) 0.039(3) Uani 1 1 d . . . . .
H11A H 0.0119 0.1224 -0.4455 0.047 Uiso 1 1 calc R U . . .
C12 C -0.1292(11) 0.1168(9) -0.3196(11) 0.045(3) Uani 1 1 d . . . . .
H12A H -0.2103 0.0667 -0.3751 0.054 Uiso 1 1 calc R U . . .
C13 C -0.1369(11) 0.1562(11) -0.1945(12) 0.045(3) Uani 1 1 d . . . . .
H13A H -0.2207 0.1281 -0.1653 0.054 Uiso 1 1 calc R U . . .
C14 C -0.0227(13) 0.2355(10) -0.1146(9) 0.042(2) Uani 1 1 d . . . . .
H14A H -0.0295 0.2634 -0.0309 0.051 Uiso 1 1 calc R U . . .
C15 C 0.1037(12) 0.2750(8) -0.1571(10) 0.046(2) Uani 1 1 d . . . . .
H15A H 0.1814 0.3299 -0.1020 0.055 Uiso 1 1 calc R U . . .
C16 C 0.1154(10) 0.2333(9) -0.2813(10) 0.036(2) Uani 1 1 d . . . . .
H16A H 0.2009 0.2603 -0.3092 0.044 Uiso 1 1 calc R U . . .
C21 C -0.3172(8) 0.3653(8) -0.3345(8) 0.0247(15) Uani 1 1 d . . . . .
C22 C -0.4356(8) 0.3052(7) -0.2962(8) 0.0281(16) Uani 1 1 d . . . . .
H22A H -0.5027 0.2422 -0.3541 0.034 Uiso 1 1 calc R U . . .
C23 C -0.4551(9) 0.3371(8) -0.1749(9) 0.0317(18) Uani 1 1 d . . . . .
H23A H -0.5311 0.2926 -0.1501 0.038 Uiso 1 1 calc R U . . .
C24 C -0.3602(13) 0.4369(11) -0.0886(11) 0.033(2) Uani 1 1 d . . . . .
H24A H -0.3732 0.4584 -0.0061 0.039 Uiso 1 1 calc R U . . .
C25 C -0.2494(9) 0.5028(8) -0.1238(7) 0.0292(16) Uani 1 1 d . . . . .
H25A H -0.1918 0.5730 -0.0665 0.035 Uiso 1 1 calc R U . . .
C26 C -0.2207(8) 0.4662(7) -0.2462(8) 0.0268(14) Uani 1 1 d . . . . .
C27 C -0.1069(8) 0.5297(7) -0.2876(8) 0.0347(16) Uani 1 1 d . . . . .
H27A H -0.0435 0.5973 -0.2318 0.042 Uiso 1 1 calc R U . . .
C28 C -0.0884(9) 0.4951(9) -0.4043(8) 0.0381(17) Uani 1 1 d . . . . .
H28A H -0.0103 0.5371 -0.4294 0.046 Uiso 1 1 calc R U . . .
C29 C -0.1837(9) 0.3967(9) -0.4908(8) 0.0394(18) Uani 1 1 d . . . . .
H29A H -0.1698 0.3755 -0.5731 0.047 Uiso 1 1 calc R U . . .
C30 C -0.2947(8) 0.3322(7) -0.4579(7) 0.0311(14) Uani 1 1 d . . . . .
H30A H -0.3567 0.2658 -0.5165 0.037 Uiso 1 1 calc R U . . .
C31 C -0.5804(14) 0.5698(11) -0.4022(10) 0.048(3) Uani 1 1 d . . . . .
H31A H -0.5746 0.5320 -0.4850 0.058 Uiso 1 1 calc R U . . .
C32 C -0.6898(10) 0.5231(9) -0.3483(10) 0.046(2) Uani 1 1 d . . . . .
H32A H -0.7612 0.4564 -0.3959 0.055 Uiso 1 1 calc R U . . .
C33 C -0.6958(10) 0.5722(10) -0.2270(11) 0.044(2) Uani 1 1 d . . . . .
H33A H -0.7697 0.5379 -0.1916 0.053 Uiso 1 1 calc R U . . .
C34 C -0.5915(13) 0.6744(10) -0.1541(10) 0.044(3) Uani 1 1 d . . . . .
H34A H -0.5934 0.7064 -0.0700 0.053 Uiso 1 1 calc R U . . .
C35 C -0.4862(10) 0.7266(8) -0.2092(11) 0.047(3) Uani 1 1 d . . . . .
H35A H -0.4200 0.7979 -0.1632 0.057 Uiso 1 1 calc R U . . .
C36 C -0.4785(12) 0.6730(11) -0.3338(12) 0.045(3) Uani 1 1 d . . . . .
H36A H -0.4054 0.7065 -0.3706 0.054 Uiso 1 1 calc R U . . .
C41 C -0.3199(14) 0.1825(12) 0.1451(11) 0.070(4) Uani 1 1 d . . . . .
C42 C -0.2765(14) -0.3504(10) 0.2930(11) 0.060(3) Uani 1 1 d . . . . .
C43 C 0.1918(14) -0.4275(8) 0.1646(9) 0.055(3) Uani 1 1 d . . . . .
C44 C 0.2206(13) 0.2638(9) 0.2881(9) 0.046(2) Uani 1 1 d . . . . .
Li1 Li -0.0408(14) -0.0719(13) 0.2520(13) 0.030(3) Uani 1 1 d . . . . .
Li2 Li 0.4509(14) -0.0871(12) 0.2232(12) 0.029(2) Uani 1 1 d . . . . .
O1 O -0.1667(8) -0.0154(10) 0.1322(9) 0.086(3) Uani 1 1 d . . . . .
O2 O -0.4365(7) -0.0457(6) 0.1046(6) 0.0437(14) Uani 1 1 d . . . . .
O3 O -0.3151(8) 0.0070(7) -0.0472(5) 0.0481(15) Uani 1 1 d . . . . .
O4 O -0.1527(7) -0.1211(7) 0.3653(6) 0.0434(15) Uani 1 1 d . . . . .
O5 O -0.4223(7) -0.1476(8) 0.3410(6) 0.0484(17) Uani 1 1 d . . . . .
O6 O -0.2699(7) -0.2014(7) 0.5073(5) 0.0473(15) Uani 1 1 d . . . . .
O7 O 0.0592(9) -0.2196(7) 0.1862(8) 0.064(2) Uani 1 1 d . . . . .
O8 O 0.0963(8) -0.3403(7) -0.0139(6) 0.0514(16) Uani 1 1 d . . . . .
O9 O 0.3034(6) -0.2221(6) 0.1305(6) 0.0453(15) Uani 1 1 d . . . . .
O10 O 0.1007(7) 0.0685(6) 0.3364(7) 0.0511(16) Uani 1 1 d . . . . .
O11 O 0.3568(9) 0.0619(7) 0.2996(8) 0.059(2) Uani 1 1 d . . . . .
O12 O 0.2956(8) 0.1995(6) 0.4835(5) 0.0510(16) Uani 1 1 d . . . . .
F1 F -0.2038(9) 0.2525(7) 0.1318(8) 0.096(3) Uani 1 1 d . . . . .
F2 F -0.3222(14) 0.2042(11) 0.2613(7) 0.150(5) Uani 1 1 d . . . . .
F3 F -0.4450(11) 0.2240(8) 0.0928(11) 0.114(3) Uani 1 1 d . . . . .
F4 F -0.1494(10) -0.4001(7) 0.3263(9) 0.093(3) Uani 1 1 d . . . . .
F5 F -0.2862(12) -0.3515(9) 0.1793(7) 0.109(3) Uani 1 1 d . . . . .
F6 F -0.3867(11) -0.4254(7) 0.3062(10) 0.109(3) Uani 1 1 d . . . . .
F7 F 0.2902(10) -0.4963(7) 0.1078(8) 0.090(3) Uani 1 1 d . . . . .
F8 F 0.0673(10) -0.5024(6) 0.1452(7) 0.082(2) Uani 1 1 d . . . . .
F9 F 0.2471(11) -0.3974(7) 0.2815(6) 0.098(3) Uani 1 1 d . . . . .
F10 F 0.1753(12) 0.2213(8) 0.1713(6) 0.097(3) Uani 1 1 d . . . . .
F11 F 0.3473(8) 0.3351(6) 0.3055(7) 0.068(2) Uani 1 1 d . . . . .
F12 F 0.1230(8) 0.3410(6) 0.3354(7) 0.075(2) Uani 1 1 d . . . . .
S1 S -0.30775(19) 0.0140(2) 0.07741(17) 0.0324(4) Uani 1 1 d . . . . .
S2 S -0.28122(18) -0.18815(18) 0.38625(16) 0.0279(3) Uani 1 1 d . . . . .
S3 S 0.15791(19) -0.28686(16) 0.10973(17) 0.0280(3) Uani 1 1 d . . . . .
S4 S 0.24654(19) 0.13318(16) 0.35939(17) 0.0279(3) 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
Re1 C13 2.206(8) . ?
Re1 C11 2.214(11) . ?
Re1 C14 2.218(9) . ?
Re1 C2 2.226(7) . ?
Re1 C15 2.227(9) . ?
Re1 C16 2.230(8) . ?
Re1 C12 2.231(9) . ?
Re1 C5 2.232(7) . ?
Re1 C3 2.238(9) . ?
Re1 C4 2.255(10) . ?
Re1 C6 2.288(7) . ?
Re1 C1 2.304(9) . ?
Re2 C22 2.215(7) . ?
Re2 C34 2.215(10) . ?
Re2 C31 2.216(10) . ?
Re2 C33 2.224(8) . ?
Re2 C36 2.231(9) . ?
Re2 C32 2.237(8) . ?
Re2 C25 2.242(8) . ?
Re2 C35 2.242(8) . ?
Re2 C23 2.243(8) . ?
Re2 C24 2.253(11) . ?
Re2 C21 2.278(8) . ?
Re2 C26 2.295(8) . ?
C1 C2 1.420(12) . ?
C1 C6 1.445(11) . ?
C1 C10 1.445(12) . ?
C2 C3 1.386(15) . ?
C2 H2A 0.9500 . ?
C3 C4 1.431(16) . ?
C3 H3A 0.9500 . ?
C4 C5 1.377(15) . ?
C4 H4A 0.9500 . ?
C5 C6 1.437(12) . ?
C5 H5A 0.9500 . ?
C6 C7 1.431(11) . ?
C7 C8 1.350(12) . ?
C7 H7A 0.9500 . ?
C8 C9 1.416(13) . ?
C8 H8A 0.9500 . ?
C9 C10 1.348(12) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C16 1.388(17) . ?
C11 C12 1.443(16) . ?
C11 H11A 0.9500 . ?
C12 C13 1.414(17) . ?
C12 H12A 0.9500 . ?
C13 C14 1.386(17) . ?
C13 H13A 0.9500 . ?
C14 C15 1.411(14) . ?
C14 H14A 0.9500 . ?
C15 C16 1.414(15) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C21 C22 1.423(10) . ?
C21 C30 1.429(11) . ?
C21 C26 1.449(10) . ?
C22 C23 1.397(13) . ?
C22 H22A 0.9500 . ?
C23 C24 1.427(15) . ?
C23 H23A 0.9500 . ?
C24 C25 1.383(14) . ?
C24 H24A 0.9500 . ?
C25 C26 1.436(12) . ?
C25 H25A 0.9500 . ?
C26 C27 1.430(10) . ?
C27 C28 1.345(12) . ?
C27 H27A 0.9500 . ?
C28 C29 1.421(13) . ?
C28 H28A 0.9500 . ?
C29 C30 1.363(11) . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9500 . ?
C31 C32 1.397(16) . ?
C31 C36 1.412(17) . ?
C31 H31A 0.9500 . ?
C32 C33 1.378(16) . ?
C32 H32A 0.9500 . ?
C33 C34 1.430(16) . ?
C33 H33A 0.9500 . ?
C34 C35 1.406(15) . ?
C34 H34A 0.9500 . ?
C35 C36 1.423(17) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C41 F2 1.309(14) . ?
C41 F1 1.330(12) . ?
C41 F3 1.349(16) . ?
C41 S1 1.799(13) . ?
C42 F5 1.304(14) . ?
C42 F6 1.320(13) . ?
C42 F4 1.333(15) . ?
C42 S2 1.810(11) . ?
C43 F7 1.321(14) . ?
C43 F9 1.324(11) . ?
C43 F8 1.327(13) . ?
C43 S3 1.806(9) . ?
C44 F10 1.309(12) . ?
C44 F12 1.317(12) . ?
C44 F11 1.325(12) . ?
C44 S4 1.811(9) . ?
Li1 O1 1.898(15) . ?
Li1 O7 1.899(14) . ?
Li1 O10 1.911(15) . ?
Li1 O4 1.940(13) . ?
Li2 O5 1.909(13) 1_655 ?
Li2 O11 1.916(14) . ?
Li2 O9 1.928(14) . ?
Li2 O2 1.961(13) 1_655 ?
O1 S1 1.423(7) . ?
O2 S1 1.432(6) . ?
O2 Li2 1.961(13) 1_455 ?
O3 S1 1.418(6) . ?
O4 S2 1.439(6) . ?
O5 S2 1.434(6) . ?
O5 Li2 1.909(13) 1_455 ?
O6 S2 1.435(6) . ?
O7 S3 1.435(7) . ?
O8 S3 1.419(7) . ?
O9 S3 1.434(6) . ?
O10 S4 1.434(6) . ?
O11 S4 1.432(7) . ?
O12 S4 1.428(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Re1 C11 68.0(4) . . ?
C13 Re1 C14 36.5(4) . . ?
C11 Re1 C14 79.3(4) . . ?
C13 Re1 C2 111.5(4) . . ?
C11 Re1 C2 112.1(4) . . ?
C14 Re1 C2 141.4(4) . . ?
C13 Re1 C15 66.3(4) . . ?
C11 Re1 C15 66.3(4) . . ?
C14 Re1 C15 37.0(4) . . ?
C2 Re1 C15 177.5(3) . . ?
C13 Re1 C16 79.0(3) . . ?
C11 Re1 C16 36.4(4) . . ?
C14 Re1 C16 66.9(3) . . ?
C2 Re1 C16 142.5(4) . . ?
C15 Re1 C16 37.0(4) . . ?
C13 Re1 C12 37.2(4) . . ?
C11 Re1 C12 37.9(4) . . ?
C14 Re1 C12 66.1(4) . . ?
C2 Re1 C12 99.6(3) . . ?
C15 Re1 C12 78.0(4) . . ?
C16 Re1 C12 66.4(4) . . ?
C13 Re1 C5 142.9(4) . . ?
C11 Re1 C5 143.6(4) . . ?
C14 Re1 C5 115.1(4) . . ?
C2 Re1 C5 78.2(3) . . ?
C15 Re1 C5 104.1(3) . . ?
C16 Re1 C5 115.8(3) . . ?
C12 Re1 C5 177.7(4) . . ?
C13 Re1 C3 100.2(4) . . ?
C11 Re1 C3 141.7(5) . . ?
C14 Re1 C3 113.5(4) . . ?
C2 Re1 C3 36.2(4) . . ?
C15 Re1 C3 144.2(4) . . ?
C16 Re1 C3 178.1(5) . . ?
C12 Re1 C3 111.9(4) . . ?
C5 Re1 C3 65.9(3) . . ?
C13 Re1 C4 113.6(4) . . ?
C11 Re1 C4 177.8(5) . . ?
C14 Re1 C4 102.9(4) . . ?
C2 Re1 C4 66.0(4) . . ?
C15 Re1 C4 115.6(4) . . ?
C16 Re1 C4 144.8(4) . . ?
C12 Re1 C4 142.7(4) . . ?
C5 Re1 C4 35.7(4) . . ?
C3 Re1 C4 37.1(4) . . ?
C13 Re1 C6 177.5(4) . . ?
C11 Re1 C6 113.2(4) . . ?
C14 Re1 C6 145.4(4) . . ?
C2 Re1 C6 66.1(3) . . ?
C15 Re1 C6 116.2(3) . . ?
C16 Re1 C6 103.2(3) . . ?
C12 Re1 C6 142.7(4) . . ?
C5 Re1 C6 37.0(3) . . ?
C3 Re1 C6 77.5(3) . . ?
C4 Re1 C6 65.2(3) . . ?
C13 Re1 C1 141.3(4) . . ?
C11 Re1 C1 100.6(4) . . ?
C14 Re1 C1 177.7(4) . . ?
C2 Re1 C1 36.5(3) . . ?
C15 Re1 C1 145.0(4) . . ?
C16 Re1 C1 114.4(3) . . ?
C12 Re1 C1 112.4(4) . . ?
C5 Re1 C1 66.3(3) . . ?
C3 Re1 C1 65.2(4) . . ?
C4 Re1 C1 77.2(3) . . ?
C6 Re1 C1 36.7(3) . . ?
C22 Re2 C34 148.9(4) . . ?
C22 Re2 C31 108.4(4) . . ?
C34 Re2 C31 79.1(4) . . ?
C22 Re2 C33 116.7(3) . . ?
C34 Re2 C33 37.6(4) . . ?
C31 Re2 C33 65.9(4) . . ?
C22 Re2 C36 136.2(4) . . ?
C34 Re2 C36 67.0(4) . . ?
C31 Re2 C36 37.0(4) . . ?
C33 Re2 C36 78.3(3) . . ?
C22 Re2 C32 101.2(3) . . ?
C34 Re2 C32 66.4(4) . . ?
C31 Re2 C32 36.6(4) . . ?
C33 Re2 C32 36.0(4) . . ?
C36 Re2 C32 66.0(4) . . ?
C22 Re2 C25 78.7(3) . . ?
C34 Re2 C25 111.3(4) . . ?
C31 Re2 C25 148.1(4) . . ?
C33 Re2 C25 139.9(4) . . ?
C36 Re2 C25 117.5(4) . . ?
C32 Re2 C25 175.2(4) . . ?
C22 Re2 C35 173.1(4) . . ?
C34 Re2 C35 36.8(4) . . ?
C31 Re2 C35 66.6(4) . . ?
C33 Re2 C35 66.3(4) . . ?
C36 Re2 C35 37.1(4) . . ?
C32 Re2 C35 77.7(3) . . ?
C25 Re2 C35 103.0(3) . . ?
C22 Re2 C23 36.5(3) . . ?
C34 Re2 C23 118.8(4) . . ?
C31 Re2 C23 136.9(4) . . ?
C33 Re2 C23 103.3(3) . . ?
C36 Re2 C23 172.5(5) . . ?
C32 Re2 C23 111.0(3) . . ?
C25 Re2 C23 66.0(3) . . ?
C35 Re2 C23 150.2(4) . . ?
C22 Re2 C24 66.2(4) . . ?
C34 Re2 C24 103.9(4) . . ?
C31 Re2 C24 173.9(5) . . ?
C33 Re2 C24 113.2(4) . . ?
C36 Re2 C24 149.1(5) . . ?
C32 Re2 C24 139.7(4) . . ?
C25 Re2 C24 35.8(4) . . ?
C35 Re2 C24 119.0(4) . . ?
C23 Re2 C24 37.0(4) . . ?
C22 Re2 C21 36.9(3) . . ?
C34 Re2 C21 174.1(4) . . ?
C31 Re2 C21 99.8(4) . . ?
C33 Re2 C21 147.1(4) . . ?
C36 Re2 C21 108.7(3) . . ?
C32 Re2 C21 116.1(3) . . ?
C25 Re2 C21 66.7(3) . . ?
C35 Re2 C21 137.5(3) . . ?
C23 Re2 C21 65.9(3) . . ?
C24 Re2 C21 77.7(4) . . ?
C22 Re2 C26 66.4(3) . . ?
C34 Re2 C26 138.5(4) . . ?
C31 Re2 C26 116.1(4) . . ?
C33 Re2 C26 175.9(4) . . ?
C36 Re2 C26 101.2(3) . . ?
C32 Re2 C26 147.4(4) . . ?
C25 Re2 C26 36.9(3) . . ?
C35 Re2 C26 110.9(3) . . ?
C23 Re2 C26 77.7(3) . . ?
C24 Re2 C26 65.2(4) . . ?
C21 Re2 C26 37.0(3) . . ?
C2 C1 C6 118.4(8) . . ?
C2 C1 C10 123.4(8) . . ?
C6 C1 C10 118.1(8) . . ?
C2 C1 Re1 68.8(5) . . ?
C6 C1 Re1 71.1(5) . . ?
C10 C1 Re1 128.6(5) . . ?
C3 C2 C1 121.4(8) . . ?
C3 C2 Re1 72.4(5) . . ?
C1 C2 Re1 74.7(4) . . ?
C3 C2 H2A 119.3 . . ?
C1 C2 H2A 119.3 . . ?
Re1 C2 H2A 125.4 . . ?
C2 C3 C4 120.1(9) . . ?
C2 C3 Re1 71.5(5) . . ?
C4 C3 Re1 72.1(5) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
Re1 C3 H3A 128.8 . . ?
C5 C4 C3 119.9(10) . . ?
C5 C4 Re1 71.2(5) . . ?
C3 C4 Re1 70.8(6) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
Re1 C4 H4A 130.6 . . ?
C4 C5 C6 121.0(8) . . ?
C4 C5 Re1 73.1(6) . . ?
C6 C5 Re1 73.6(4) . . ?
C4 C5 H5A 119.5 . . ?
C6 C5 H5A 119.5 . . ?
Re1 C5 H5A 125.7 . . ?
C7 C6 C5 122.9(8) . . ?
C7 C6 C1 118.2(8) . . ?
C5 C6 C1 118.8(8) . . ?
C7 C6 Re1 128.1(5) . . ?
C5 C6 Re1 69.4(4) . . ?
C1 C6 Re1 72.3(5) . . ?
C8 C7 C6 121.1(8) . . ?
C8 C7 H7A 119.5 . . ?
C6 C7 H7A 119.5 . . ?
C7 C8 C9 121.1(8) . . ?
C7 C8 H8A 119.5 . . ?
C9 C8 H8A 119.5 . . ?
C10 C9 C8 120.8(8) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?
C9 C10 C1 120.8(8) . . ?
C9 C10 H10A 119.6 . . ?
C1 C10 H10A 119.6 . . ?
C16 C11 C12 119.3(11) . . ?
C16 C11 Re1 72.4(6) . . ?
C12 C11 Re1 71.7(6) . . ?
C16 C11 H11A 120.4 . . ?
C12 C11 H11A 120.4 . . ?
Re1 C11 H11A 127.5 . . ?
C13 C12 C11 119.6(10) . . ?
C13 C12 Re1 70.5(5) . . ?
C11 C12 Re1 70.4(6) . . ?
C13 C12 H12A 120.2 . . ?
C11 C12 H12A 120.2 . . ?
Re1 C12 H12A 131.8 . . ?
C14 C13 C12 120.2(9) . . ?
C14 C13 Re1 72.2(5) . . ?
C12 C13 Re1 72.4(5) . . ?
C14 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
Re1 C13 H13A 127.6 . . ?
C13 C14 C15 120.2(9) . . ?
C13 C14 Re1 71.3(6) . . ?
C15 C14 Re1 71.9(5) . . ?
C13 C14 H14A 119.9 . . ?
C15 C14 H14A 119.9 . . ?
Re1 C14 H14A 129.3 . . ?
C14 C15 C16 120.4(9) . . ?
C14 C15 Re1 71.1(5) . . ?
C16 C15 Re1 71.6(5) . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 H15A 119.8 . . ?
Re1 C15 H15A 130.0 . . ?
C11 C16 C15 120.2(9) . . ?
C11 C16 Re1 71.2(6) . . ?
C15 C16 Re1 71.4(5) . . ?
C11 C16 H16A 119.9 . . ?
C15 C16 H16A 119.9 . . ?
Re1 C16 H16A 130.1 . . ?
C22 C21 C30 121.8(7) . . ?
C22 C21 C26 118.7(8) . . ?
C30 C21 C26 119.5(7) . . ?
C22 C21 Re2 69.1(4) . . ?
C30 C21 Re2 128.5(5) . . ?
C26 C21 Re2 72.2(5) . . ?
C23 C22 C21 121.2(7) . . ?
C23 C22 Re2 72.8(5) . . ?
C21 C22 Re2 74.0(5) . . ?
C23 C22 H22A 119.4 . . ?
C21 C22 H22A 119.4 . . ?
Re2 C22 H22A 125.6 . . ?
C22 C23 C24 119.7(8) . . ?
C22 C23 Re2 70.7(5) . . ?
C24 C23 Re2 71.9(6) . . ?
C22 C23 H23A 120.2 . . ?
C24 C23 H23A 120.2 . . ?
Re2 C23 H23A 129.7 . . ?
C25 C24 C23 120.7(10) . . ?
C25 C24 Re2 71.6(6) . . ?
C23 C24 Re2 71.1(6) . . ?
C25 C24 H24A 119.7 . . ?
C23 C24 H24A 119.7 . . ?
Re2 C24 H24A 130.2 . . ?
C24 C25 C26 120.7(8) . . ?
C24 C25 Re2 72.5(6) . . ?
C26 C25 Re2 73.6(4) . . ?
C24 C25 H25A 119.7 . . ?
C26 C25 H25A 119.7 . . ?
Re2 C25 H25A 126.1 . . ?
C27 C26 C25 123.2(7) . . ?
C27 C26 C21 117.8(8) . . ?
C25 C26 C21 118.8(7) . . ?
C27 C26 Re2 128.4(5) . . ?
C25 C26 Re2 69.5(5) . . ?
C21 C26 Re2 70.9(4) . . ?
C28 C27 C26 121.0(8) . . ?
C28 C27 H27A 119.5 . . ?
C26 C27 H27A 119.5 . . ?
C27 C28 C29 121.0(8) . . ?
C27 C28 H28A 119.5 . . ?
C29 C28 H28A 119.5 . . ?
C30 C29 C28 121.3(8) . . ?
C30 C29 H29A 119.4 . . ?
C28 C29 H29A 119.4 . . ?
C29 C30 C21 119.4(7) . . ?
C29 C30 H30A 120.3 . . ?
C21 C30 H30A 120.3 . . ?
C32 C31 C36 120.0(10) . . ?
C32 C31 Re2 72.5(6) . . ?
C36 C31 Re2 72.1(6) . . ?
C32 C31 H31A 120.0 . . ?
C36 C31 H31A 120.0 . . ?
Re2 C31 H31A 127.4 . . ?
C33 C32 C31 121.0(9) . . ?
C33 C32 Re2 71.5(5) . . ?
C31 C32 Re2 70.9(6) . . ?
C33 C32 H32A 119.5 . . ?
C31 C32 H32A 119.5 . . ?
Re2 C32 H32A 130.9 . . ?
C32 C33 C34 120.5(9) . . ?
C32 C33 Re2 72.5(5) . . ?
C34 C33 Re2 70.9(5) . . ?
C32 C33 H33A 119.7 . . ?
C34 C33 H33A 119.7 . . ?
Re2 C33 H33A 129.3 . . ?
C35 C34 C33 118.8(10) . . ?
C35 C34 Re2 72.6(5) . . ?
C33 C34 Re2 71.5(6) . . ?
C35 C34 H34A 120.6 . . ?
C33 C34 H34A 120.6 . . ?
Re2 C34 H34A 127.2 . . ?
C34 C35 C36 120.2(9) . . ?
C34 C35 Re2 70.6(5) . . ?
C36 C35 Re2 71.0(5) . . ?
C34 C35 H35A 119.9 . . ?
C36 C35 H35A 119.9 . . ?
Re2 C35 H35A 131.2 . . ?
C31 C36 C35 119.4(9) . . ?
C31 C36 Re2 70.9(6) . . ?
C35 C36 Re2 71.9(5) . . ?
C31 C36 H36A 120.3 . . ?
C35 C36 H36A 120.3 . . ?
Re2 C36 H36A 129.2 . . ?
F2 C41 F1 107.5(10) . . ?
F2 C41 F3 108.8(12) . . ?
F1 C41 F3 107.8(12) . . ?
F2 C41 S1 110.7(11) . . ?
F1 C41 S1 111.5(9) . . ?
F3 C41 S1 110.3(8) . . ?
F5 C42 F6 109.5(11) . . ?
F5 C42 F4 108.5(11) . . ?
F6 C42 F4 107.1(10) . . ?
F5 C42 S2 110.7(8) . . ?
F6 C42 S2 110.6(9) . . ?
F4 C42 S2 110.4(8) . . ?
F7 C43 F9 106.6(10) . . ?
F7 C43 F8 107.5(8) . . ?
F9 C43 F8 108.7(9) . . ?
F7 C43 S3 110.5(7) . . ?
F9 C43 S3 112.3(6) . . ?
F8 C43 S3 111.0(8) . . ?
F10 C44 F12 108.7(9) . . ?
F10 C44 F11 108.0(10) . . ?
F12 C44 F11 106.5(8) . . ?
F10 C44 S4 111.7(7) . . ?
F12 C44 S4 111.1(7) . . ?
F11 C44 S4 110.6(7) . . ?
O1 Li1 O7 113.0(8) . . ?
O1 Li1 O10 106.9(7) . . ?
O7 Li1 O10 110.3(7) . . ?
O1 Li1 O4 111.7(7) . . ?
O7 Li1 O4 105.3(7) . . ?
O10 Li1 O4 109.6(8) . . ?
O5 Li2 O11 110.6(7) 1_655 . ?
O5 Li2 O9 109.8(7) 1_655 . ?
O11 Li2 O9 110.7(7) . . ?
O5 Li2 O2 111.0(7) 1_655 1_655 ?
O11 Li2 O2 109.5(6) . 1_655 ?
O9 Li2 O2 105.1(7) . 1_655 ?
S1 O1 Li1 153.0(7) . . ?
S1 O2 Li2 150.1(6) . 1_455 ?
S2 O4 Li1 149.0(7) . . ?
S2 O5 Li2 151.4(6) . 1_455 ?
S3 O7 Li1 152.7(6) . . ?
S3 O9 Li2 151.0(6) . . ?
S4 O10 Li1 151.6(6) . . ?
S4 O11 Li2 157.2(6) . . ?
O3 S1 O1 113.3(5) . . ?
O3 S1 O2 113.7(4) . . ?
O1 S1 O2 116.2(4) . . ?
O3 S1 C41 103.2(5) . . ?
O1 S1 C41 104.9(6) . . ?
O2 S1 C41 103.7(5) . . ?
O5 S2 O6 114.0(4) . . ?
O5 S2 O4 114.9(4) . . ?
O6 S2 O4 113.8(4) . . ?
O5 S2 C42 104.2(5) . . ?
O6 S2 C42 104.6(5) . . ?
O4 S2 C42 103.6(5) . . ?
O8 S3 O9 114.9(4) . . ?
O8 S3 O7 116.5(5) . . ?
O9 S3 O7 113.5(5) . . ?
O8 S3 C43 102.9(4) . . ?
O9 S3 C43 103.6(5) . . ?
O7 S3 C43 103.1(5) . . ?
O12 S4 O11 115.1(5) . . ?
O12 S4 O10 113.8(4) . . ?
O11 S4 O10 115.6(5) . . ?
O12 S4 C44 102.5(4) . . ?
O11 S4 C44 103.5(4) . . ?
O10 S4 C44 104.0(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
C6 C1 C2 C3 -4.9(11) . . . . ?
C10 C1 C2 C3 179.3(8) . . . . ?
Re1 C1 C2 C3 -57.7(7) . . . . ?
C6 C1 C2 Re1 52.7(6) . . . . ?
C10 C1 C2 Re1 -123.0(7) . . . . ?
C1 C2 C3 C4 3.5(12) . . . . ?
Re1 C2 C3 C4 -55.3(8) . . . . ?
C1 C2 C3 Re1 58.8(7) . . . . ?
C2 C3 C4 C5 1.4(14) . . . . ?
Re1 C3 C4 C5 -53.5(8) . . . . ?
C2 C3 C4 Re1 55.0(7) . . . . ?
C3 C4 C5 C6 -4.8(13) . . . . ?
Re1 C4 C5 C6 -58.1(7) . . . . ?
C3 C4 C5 Re1 53.3(8) . . . . ?
C4 C5 C6 C7 -179.4(8) . . . . ?
Re1 C5 C6 C7 122.8(7) . . . . ?
C4 C5 C6 C1 3.2(11) . . . . ?
Re1 C5 C6 C1 -54.6(6) . . . . ?
C4 C5 C6 Re1 57.9(7) . . . . ?
C2 C1 C6 C7 -175.9(7) . . . . ?
C10 C1 C6 C7 0.1(10) . . . . ?
Re1 C1 C6 C7 -124.3(6) . . . . ?
C2 C1 C6 C5 1.6(10) . . . . ?
C10 C1 C6 C5 177.6(7) . . . . ?
Re1 C1 C6 C5 53.3(6) . . . . ?
C2 C1 C6 Re1 -51.7(6) . . . . ?
C10 C1 C6 Re1 124.3(7) . . . . ?
C5 C6 C7 C8 -178.0(7) . . . . ?
C1 C6 C7 C8 -0.6(10) . . . . ?
Re1 C6 C7 C8 -89.5(9) . . . . ?
C6 C7 C8 C9 0.3(11) . . . . ?
C7 C8 C9 C10 0.7(12) . . . . ?
C8 C9 C10 C1 -1.2(11) . . . . ?
C2 C1 C10 C9 176.6(7) . . . . ?
C6 C1 C10 C9 0.8(11) . . . . ?
Re1 C1 C10 C9 88.3(9) . . . . ?
C16 C11 C12 C13 -4.3(14) . . . . ?
Re1 C11 C12 C13 52.4(8) . . . . ?
C16 C11 C12 Re1 -56.6(9) . . . . ?
C11 C12 C13 C14 3.9(14) . . . . ?
Re1 C12 C13 C14 56.2(8) . . . . ?
C11 C12 C13 Re1 -52.3(8) . . . . ?
C12 C13 C14 C15 -1.5(14) . . . . ?
Re1 C13 C14 C15 54.8(8) . . . . ?
C12 C13 C14 Re1 -56.3(8) . . . . ?
C13 C14 C15 C16 -0.5(14) . . . . ?
Re1 C14 C15 C16 54.0(8) . . . . ?
C13 C14 C15 Re1 -54.5(8) . . . . ?
C12 C11 C16 C15 2.3(15) . . . . ?
Re1 C11 C16 C15 -54.0(8) . . . . ?
C12 C11 C16 Re1 56.3(8) . . . . ?
C14 C15 C16 C11 0.0(14) . . . . ?
Re1 C15 C16 C11 53.8(8) . . . . ?
C14 C15 C16 Re1 -53.8(8) . . . . ?
C30 C21 C22 C23 179.1(7) . . . . ?
C26 C21 C22 C23 -3.3(11) . . . . ?
Re2 C21 C22 C23 -57.7(7) . . . . ?
C30 C21 C22 Re2 -123.2(7) . . . . ?
C26 C21 C22 Re2 54.4(7) . . . . ?
C21 C22 C23 C24 3.7(13) . . . . ?
Re2 C22 C23 C24 -54.6(8) . . . . ?
C21 C22 C23 Re2 58.3(7) . . . . ?
C22 C23 C24 C25 0.2(15) . . . . ?
Re2 C23 C24 C25 -53.8(9) . . . . ?
C22 C23 C24 Re2 54.0(8) . . . . ?
C23 C24 C25 C26 -4.4(15) . . . . ?
Re2 C24 C25 C26 -57.9(7) . . . . ?
C23 C24 C25 Re2 53.5(9) . . . . ?
C24 C25 C26 C27 -179.4(8) . . . . ?
Re2 C25 C26 C27 123.2(7) . . . . ?
C24 C25 C26 C21 4.6(12) . . . . ?
Re2 C25 C26 C21 -52.8(7) . . . . ?
C24 C25 C26 Re2 57.4(8) . . . . ?
C22 C21 C26 C27 -177.0(6) . . . . ?
C30 C21 C26 C27 0.6(11) . . . . ?
Re2 C21 C26 C27 -124.1(7) . . . . ?
C22 C21 C26 C25 -0.8(11) . . . . ?
C30 C21 C26 C25 176.9(7) . . . . ?
Re2 C21 C26 C25 52.2(7) . . . . ?
C22 C21 C26 Re2 -53.0(6) . . . . ?
C30 C21 C26 Re2 124.7(7) . . . . ?
C25 C26 C27 C28 -177.3(8) . . . . ?
C21 C26 C27 C28 -1.2(11) . . . . ?
Re2 C26 C27 C28 -88.1(9) . . . . ?
C26 C27 C28 C29 1.7(12) . . . . ?
C27 C28 C29 C30 -1.5(13) . . . . ?
C28 C29 C30 C21 0.9(12) . . . . ?
C22 C21 C30 C29 177.1(7) . . . . ?
C26 C21 C30 C29 -0.5(11) . . . . ?
Re2 C21 C30 C29 89.5(8) . . . . ?
C36 C31 C32 C33 -3.2(14) . . . . ?
Re2 C31 C32 C33 53.2(8) . . . . ?
C36 C31 C32 Re2 -56.3(9) . . . . ?
C31 C32 C33 C34 1.3(14) . . . . ?
Re2 C32 C33 C34 54.2(8) . . . . ?
C31 C32 C33 Re2 -52.9(8) . . . . ?
C32 C33 C34 C35 2.1(14) . . . . ?
Re2 C33 C34 C35 57.1(8) . . . . ?
C32 C33 C34 Re2 -55.0(8) . . . . ?
C33 C34 C35 C36 -3.7(14) . . . . ?
Re2 C34 C35 C36 52.9(8) . . . . ?
C33 C34 C35 Re2 -56.6(8) . . . . ?
C32 C31 C36 C35 1.5(15) . . . . ?
Re2 C31 C36 C35 -55.1(8) . . . . ?
C32 C31 C36 Re2 56.6(8) . . . . ?
C34 C35 C36 C31 1.9(14) . . . . ?
Re2 C35 C36 C31 54.6(8) . . . . ?
C34 C35 C36 Re2 -52.7(8) . . . . ?
O7 Li1 O1 S1 120.0(18) . . . . ?
O10 Li1 O1 S1 -118.4(18) . . . . ?
O4 Li1 O1 S1 1(2) . . . . ?
O1 Li1 O7 S3 59.5(19) . . . . ?
O10 Li1 O7 S3 -60.1(19) . . . . ?
O4 Li1 O7 S3 -178.3(14) . . . . ?
Li1 O1 S1 O3 -155.8(18) . . . . ?
Li1 O1 S1 O2 -21(2) . . . . ?
Li1 O1 S1 C41 92(2) . . . . ?
Li2 O2 S1 O3 -175.5(11) 1_455 . . . ?
Li2 O2 S1 O1 50.4(13) 1_455 . . . ?
Li2 O2 S1 C41 -64.2(13) 1_455 . . . ?
F2 C41 S1 O3 176.8(9) . . . . ?
F1 C41 S1 O3 -63.5(10) . . . . ?
F3 C41 S1 O3 56.3(9) . . . . ?
F2 C41 S1 O1 -64.3(10) . . . . ?
F1 C41 S1 O1 55.4(11) . . . . ?
F3 C41 S1 O1 175.2(8) . . . . ?
F2 C41 S1 O2 58.0(10) . . . . ?
F1 C41 S1 O2 177.7(9) . . . . ?
F3 C41 S1 O2 -62.5(9) . . . . ?
Li2 O5 S2 O6 169.6(13) 1_455 . . . ?
Li2 O5 S2 O4 35.7(16) 1_455 . . . ?
Li2 O5 S2 C42 -77.0(15) 1_455 . . . ?
Li1 O4 S2 O5 -58.6(13) . . . . ?
Li1 O4 S2 O6 167.5(11) . . . . ?
Li1 O4 S2 C42 54.5(13) . . . . ?
F5 C42 S2 O5 60.0(10) . . . . ?
F6 C42 S2 O5 -61.6(10) . . . . ?
F4 C42 S2 O5 -179.8(8) . . . . ?
F5 C42 S2 O6 180.0(9) . . . . ?
F6 C42 S2 O6 58.4(10) . . . . ?
F4 C42 S2 O6 -59.9(9) . . . . ?
F5 C42 S2 O4 -60.6(10) . . . . ?
F6 C42 S2 O4 177.9(9) . . . . ?
F4 C42 S2 O4 59.6(9) . . . . ?
Li2 O9 S3 O8 146.3(11) . . . . ?
Li2 O9 S3 O7 8.8(13) . . . . ?
Li2 O9 S3 C43 -102.3(12) . . . . ?
Li1 O7 S3 O8 -82.4(17) . . . . ?
Li1 O7 S3 O9 54.4(18) . . . . ?
Li1 O7 S3 C43 165.7(16) . . . . ?
F7 C43 S3 O8 62.6(8) . . . . ?
F9 C43 S3 O8 -178.4(9) . . . . ?
F8 C43 S3 O8 -56.5(8) . . . . ?
F7 C43 S3 O9 -57.3(8) . . . . ?
F9 C43 S3 O9 61.6(10) . . . . ?
F8 C43 S3 O9 -176.4(7) . . . . ?
F7 C43 S3 O7 -175.8(7) . . . . ?
F9 C43 S3 O7 -56.9(10) . . . . ?
F8 C43 S3 O7 65.1(8) . . . . ?
Li2 O11 S4 O12 110.5(18) . . . . ?
Li2 O11 S4 O10 -25(2) . . . . ?
Li2 O11 S4 C44 -138.4(18) . . . . ?
Li1 O10 S4 O12 -144.5(13) . . . . ?
Li1 O10 S4 O11 -7.9(15) . . . . ?
Li1 O10 S4 C44 104.8(13) . . . . ?
F10 C44 S4 O12 179.7(8) . . . . ?
F12 C44 S4 O12 -58.7(9) . . . . ?
F11 C44 S4 O12 59.4(8) . . . . ?
F10 C44 S4 O11 59.7(10) . . . . ?
F12 C44 S4 O11 -178.7(8) . . . . ?
F11 C44 S4 O11 -60.7(8) . . . . ?
F10 C44 S4 O10 -61.5(9) . . . . ?
F12 C44 S4 O10 60.1(9) . . . . ?
F11 C44 S4 O10 178.1(7) . . . . ?

_refine_diff_density_max         1.219
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.138

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_GIM210616
_database_code_depnum_ccdc_archive 'CCDC 1554397'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H16 B N6 Re'
_chemical_formula_weight         477.35

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'
B B 0.0013 0.0007 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.2517(4)
_cell_length_b                   10.2422(6)
_cell_length_c                   8.9263(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.507(5)
_cell_angle_gamma                90
_cell_volume                     753.69(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    4135
_cell_measurement_theta_min      2.9820
_cell_measurement_theta_max      32.2970

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_F_000             456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    8.069
_shelx_estimated_absorpt_T_min   0.444
_shelx_estimated_absorpt_T_max   0.738
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Oxford Xcalibur Ruby CCD'
_diffrn_measurement_method       'ο oscillation scan'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            9097
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.284
_diffrn_reflns_theta_max         32.874
_diffrn_reflns_theta_full        26.32
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2736
_reflns_number_gt                2473
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro (Oxford, 2007)'
_computing_cell_refinement       'CrysAlisPro (Oxford, 2007)'
_computing_data_reduction        'CrysAlisPro (Oxford, 2007)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0237P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2736
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0722
_refine_ls_wR_factor_gt          0.0691
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.15231(2) 0.2500 0.51808(2) 0.01627(7) Uani 1 2 d S T P . .
C1 C 0.0053(7) 0.2500 0.3086(6) 0.0320(15) Uani 1 2 d S T P . .
H1A H -0.1095 0.2500 0.2947 0.038 Uiso 1 2 calc R U P . .
C2 C 0.0887(6) 0.1287(5) 0.3186(4) 0.0322(10) Uani 1 1 d . . . . .
H2A H 0.0320 0.0484 0.3067 0.039 Uiso 1 1 calc R U . . .
C3 C 0.2596(5) 0.1311(4) 0.3472(4) 0.0269(9) Uani 1 1 d . . . . .
H3A H 0.3166 0.0509 0.3596 0.032 Uiso 1 1 calc R U . . .
C4 C 0.3470(7) 0.2500 0.3576(7) 0.0295(14) Uani 1 2 d S T P . .
H4A H 0.4618 0.2500 0.3714 0.035 Uiso 1 2 calc R U P . .
C5 C -0.2249(7) 0.2500 0.5964(8) 0.0317(14) Uani 1 2 d S T P . .
H5A H -0.2650 0.2500 0.4950 0.038 Uiso 1 2 calc R U P . .
C6 C -0.3210(8) 0.2500 0.7208(8) 0.0362(17) Uani 1 2 d S T P . .
H6A H -0.4361 0.2500 0.7206 0.043 Uiso 1 2 calc R U P . .
C7 C -0.2149(8) 0.2500 0.8440(8) 0.0334(15) Uani 1 2 d S T P . .
H7A H -0.2438 0.2500 0.9459 0.040 Uiso 1 2 calc R U P . .
C8 C 0.3294(4) 0.0077(4) 0.6884(5) 0.0233(8) Uani 1 1 d . . . . .
H8 H 0.3724 -0.0280 0.6003 0.028 Uiso 1 1 calc R U . . .
C9 C 0.3563(5) -0.0429(4) 0.8314(5) 0.0286(9) Uani 1 1 d . . . . .
H9 H 0.4206 -0.1164 0.8603 0.034 Uiso 1 1 calc R U . . .
C10 C 0.2694(5) 0.0368(4) 0.9217(5) 0.0292(9) Uani 1 1 d . . . . .
H10 H 0.2619 0.0278 1.0271 0.035 Uiso 1 1 calc R U . . .
B1 B 0.1004(9) 0.2500 0.8824(7) 0.0259(14) Uani 1 2 d S T P . .
H11 H 0.079(8) 0.2500 0.999(7) 0.039 Uiso 1 2 d S U P . .
N1 N -0.0673(5) 0.2500 0.6410(5) 0.0217(10) Uani 1 2 d S T P . .
N2 N -0.0625(6) 0.2500 0.7947(5) 0.0241(10) Uani 1 2 d S T P . .
N3 N 0.2353(4) 0.1126(3) 0.6912(4) 0.0201(6) Uani 1 1 d . . . . .
N4 N 0.1968(4) 0.1296(4) 0.8368(3) 0.0232(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
Re1 N1 2.159(4) . ?
Re1 C3 2.171(4) . ?
Re1 C3 2.171(4) 4_565 ?
Re1 N3 2.178(3) 4_565 ?
Re1 N3 2.178(3) . ?
Re1 C1 2.184(6) . ?
Re1 C4 2.198(5) . ?
Re1 C2 2.215(4) 4_565 ?
Re1 C2 2.215(4) . ?
C1 C2 1.421(6) . ?
C1 C2 1.421(6) 4_565 ?
C1 H1A 0.9500 . ?
C2 C3 1.422(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.416(5) . ?
C3 H3A 0.9500 . ?
C4 C3 1.416(5) 4_565 ?
C4 H4A 0.9500 . ?
C5 N1 1.344(8) . ?
C5 C6 1.391(8) . ?
C5 H5A 0.9500 . ?
C6 C7 1.376(10) . ?
C6 H6A 0.9500 . ?
C7 N2 1.351(7) . ?
C7 H7A 0.9500 . ?
C8 N3 1.327(5) . ?
C8 C9 1.386(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.372(6) . ?
C9 H9 0.9500 . ?
C10 N4 1.340(5) . ?
C10 H10 0.9500 . ?
B1 N2 1.526(9) . ?
B1 N4 1.532(5) . ?
B1 N4 1.532(5) 4_565 ?
B1 H11 1.06(6) . ?
N1 N2 1.371(6) . ?
N3 N4 1.362(4) . ?

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
N1 Re1 C3 137.24(14) . . ?
N1 Re1 C3 137.24(14) . 4_565 ?
C3 Re1 C3 68.3(2) . 4_565 ?
N1 Re1 N3 83.34(13) . 4_565 ?
C3 Re1 N3 137.38(14) . 4_565 ?
C3 Re1 N3 90.64(14) 4_565 4_565 ?
N1 Re1 N3 83.34(13) . . ?
C3 Re1 N3 90.64(14) . . ?
C3 Re1 N3 137.38(14) 4_565 . ?
N3 Re1 N3 80.46(18) 4_565 . ?
N1 Re1 C1 89.3(2) . . ?
C3 Re1 C1 68.07(16) . . ?
C3 Re1 C1 68.07(16) 4_565 . ?
N3 Re1 C1 138.86(9) 4_565 . ?
N3 Re1 C1 138.86(9) . . ?
N1 Re1 C4 169.9(2) . . ?
C3 Re1 C4 37.82(13) . . ?
C3 Re1 C4 37.82(13) 4_565 . ?
N3 Re1 C4 104.27(15) 4_565 . ?
N3 Re1 C4 104.27(15) . . ?
C1 Re1 C4 80.6(2) . . ?
N1 Re1 C2 103.51(16) . 4_565 ?
C3 Re1 C2 80.77(16) . 4_565 ?
C3 Re1 C2 37.83(17) 4_565 4_565 ?
N3 Re1 C2 105.31(17) 4_565 4_565 ?
N3 Re1 C2 171.37(13) . 4_565 ?
C1 Re1 C2 37.69(15) . 4_565 ?
C4 Re1 C2 68.32(18) . 4_565 ?
N1 Re1 C2 103.51(16) . . ?
C3 Re1 C2 37.83(17) . . ?
C3 Re1 C2 80.77(16) 4_565 . ?
N3 Re1 C2 171.37(13) 4_565 . ?
N3 Re1 C2 105.31(17) . . ?
C1 Re1 C2 37.69(15) . . ?
C4 Re1 C2 68.32(18) . . ?
C2 Re1 C2 68.2(3) 4_565 . ?
C2 C1 C2 121.9(5) . 4_565 ?
C2 C1 Re1 72.3(3) . . ?
C2 C1 Re1 72.3(3) 4_565 . ?
C2 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 4_565 . ?
Re1 C1 H1A 128.7 . . ?
C1 C2 C3 118.0(4) . . ?
C1 C2 Re1 70.0(3) . . ?
C3 C2 Re1 69.4(2) . . ?
C1 C2 H2A 121.0 . . ?
C3 C2 H2A 121.0 . . ?
Re1 C2 H2A 132.4 . . ?
C4 C3 C2 121.6(4) . . ?
C4 C3 Re1 72.1(3) . . ?
C2 C3 Re1 72.8(2) . . ?
C4 C3 H3A 119.2 . . ?
C2 C3 H3A 119.2 . . ?
Re1 C3 H3A 128.2 . . ?
C3 C4 C3 118.6(5) . 4_565 ?
C3 C4 Re1 70.0(3) . . ?
C3 C4 Re1 70.0(3) 4_565 . ?
C3 C4 H4A 120.7 . . ?
C3 C4 H4A 120.7 4_565 . ?
Re1 C4 H4A 132.0 . . ?
N1 C5 C6 110.0(6) . . ?
N1 C5 H5A 125.0 . . ?
C6 C5 H5A 125.0 . . ?
C7 C6 C5 105.9(5) . . ?
C7 C6 H6A 127.1 . . ?
C5 C6 H6A 127.1 . . ?
N2 C7 C6 107.9(5) . . ?
N2 C7 H7A 126.0 . . ?
C6 C7 H7A 126.0 . . ?
N3 C8 C9 110.8(4) . . ?
N3 C8 H8 124.6 . . ?
C9 C8 H8 124.6 . . ?
C10 C9 C8 104.6(4) . . ?
C10 C9 H9 127.7 . . ?
C8 C9 H9 127.7 . . ?
N4 C10 C9 108.8(4) . . ?
N4 C10 H10 125.6 . . ?
C9 C10 H10 125.6 . . ?
N2 B1 N4 108.6(3) . . ?
N2 B1 N4 108.6(3) . 4_565 ?
N4 B1 N4 107.2(5) . 4_565 ?
N2 B1 H11 109(4) . . ?
N4 B1 H11 112(2) . . ?
N4 B1 H11 112(2) 4_565 . ?
C5 N1 N2 106.3(5) . . ?
C5 N1 Re1 132.3(4) . . ?
N2 N1 Re1 121.4(3) . . ?
C7 N2 N1 109.9(5) . . ?
C7 N2 B1 130.1(5) . . ?
N1 N2 B1 120.0(4) . . ?
C8 N3 N4 106.4(3) . . ?
C8 N3 Re1 132.5(3) . . ?
N4 N3 Re1 121.0(3) . . ?
C10 N4 N3 109.4(3) . . ?
C10 N4 B1 130.1(4) . . ?
N3 N4 B1 120.1(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 C2 C3 3.2(8) 4_565 . . . ?
Re1 C1 C2 C3 -51.8(4) . . . . ?
C2 C1 C2 Re1 55.0(5) 4_565 . . . ?
C1 C2 C3 C4 -3.3(6) . . . . ?
Re1 C2 C3 C4 -55.4(4) . . . . ?
C1 C2 C3 Re1 52.1(4) . . . . ?
C2 C3 C4 C3 3.4(8) . . . 4_565 ?
Re1 C3 C4 C3 -52.3(5) . . . 4_565 ?
C2 C3 C4 Re1 55.7(4) . . . . ?
N1 C5 C6 C7 0.000(2) . . . . ?
C5 C6 C7 N2 0.000(2) . . . . ?
N3 C8 C9 C10 1.2(5) . . . . ?
C8 C9 C10 N4 -0.5(5) . . . . ?
C6 C5 N1 N2 0.000(1) . . . . ?
C6 C5 N1 Re1 180.000(1) . . . . ?
C6 C7 N2 N1 0.000(2) . . . . ?
C6 C7 N2 B1 180.000(2) . . . . ?
C5 N1 N2 C7 0.000(2) . . . . ?
Re1 N1 N2 C7 180.000(2) . . . . ?
C5 N1 N2 B1 180.000(2) . . . . ?
Re1 N1 N2 B1 0.000(2) . . . . ?
N4 B1 N2 C7 121.9(3) . . . . ?
N4 B1 N2 C7 -121.9(3) 4_565 . . . ?
N4 B1 N2 N1 -58.1(3) . . . . ?
N4 B1 N2 N1 58.1(3) 4_565 . . . ?
C9 C8 N3 N4 -1.4(5) . . . . ?
C9 C8 N3 Re1 175.8(3) . . . . ?
C9 C10 N4 N3 -0.3(5) . . . . ?
C9 C10 N4 B1 -173.2(4) . . . . ?
C8 N3 N4 C10 1.0(4) . . . . ?
Re1 N3 N4 C10 -176.6(3) . . . . ?
C8 N3 N4 B1 174.7(4) . . . . ?
Re1 N3 N4 B1 -2.8(5) . . . . ?
N2 B1 N4 C10 -128.0(5) . . . . ?
N4 B1 N4 C10 114.8(5) 4_565 . . . ?
N2 B1 N4 N3 59.7(5) . . . . ?
N4 B1 N4 N3 -57.5(6) 4_565 . . . ?

_refine_diff_density_max         2.324
_refine_diff_density_min         -2.491
_refine_diff_density_rms         0.220

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_GIM140616
_database_code_depnum_ccdc_archive 'CCDC 1554398'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21.90 H33 F2.70 N3 O3.10 Re1.10 S0.90'
_chemical_formula_weight         672.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7977(5)
_cell_length_b                   10.9136(7)
_cell_length_c                   13.8305(6)
_cell_angle_alpha                104.511(5)
_cell_angle_beta                 109.525(4)
_cell_angle_gamma                93.636(5)
_cell_volume                     1331.70(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    27915
_cell_measurement_theta_min      2.8780
_cell_measurement_theta_max      37.9030

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_F_000             663
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    5.130
_shelx_estimated_absorpt_T_min   0.308
_shelx_estimated_absorpt_T_max   0.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.57410
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Oxford Xcalibur Ruby CCD'
_diffrn_measurement_method       'ο oscillation scan'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            55166
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.153
_diffrn_reflns_theta_max         36.318
_diffrn_reflns_theta_full        36.23
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12802
_reflns_number_gt                11886
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro (Oxford, 2007)'
_computing_cell_refinement       'CrysAlisPro (Oxford, 2007)'
_computing_data_reduction        'CrysAlisPro (Oxford, 2007)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0345P)²+0.5259P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12802
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0683
_refine_ls_wR_factor_gt          0.0662
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.17584(2) 0.14619(2) 0.32895(2) 0.01845(2) Uani 1 1 d . . . . .
Re2 Re 0.80449(13) -0.45580(10) 0.24436(8) 0.02735(17) Uani 0.1 1 d . . P A 2
C1 C -0.0679(3) 0.0734(4) 0.2565(3) 0.0565(10) Uani 1 1 d . . . . .
H1 H -0.1290 0.0344 0.1838 0.068 Uiso 1 1 calc R U . . .
C2 C 0.0004(4) -0.0011(3) 0.3214(4) 0.0619(12) Uani 1 1 d . . . . .
H2 H -0.0103 -0.0912 0.2916 0.074 Uiso 1 1 calc R U . . .
C3 C 0.0842(4) 0.0553(4) 0.4296(3) 0.0529(9) Uani 1 1 d . . . . .
H3 H 0.1272 0.0037 0.4740 0.063 Uiso 1 1 calc R U . . .
C4 C 0.1042(3) 0.1861(4) 0.4713(2) 0.0467(7) Uani 1 1 d . . . . .
H4 H 0.1643 0.2245 0.5444 0.056 Uiso 1 1 calc R U . . .
C5 C 0.0379(3) 0.2639(3) 0.4087(3) 0.0435(7) Uani 1 1 d . . . . .
H5 H 0.0492 0.3538 0.4396 0.052 Uiso 1 1 calc R U . . .
C6 C -0.0446(3) 0.2079(4) 0.3010(3) 0.0466(7) Uani 1 1 d . . . . .
H6 H -0.0856 0.2603 0.2568 0.056 Uiso 1 1 calc R U . . .
C7 C 0.2811(2) 0.0158(2) 0.27014(19) 0.0264(4) Uani 1 1 d . . . . .
C8 C 0.3786(2) 0.2358(2) 0.42154(17) 0.0243(3) Uani 1 1 d . . . . .
C9 C 0.1901(2) 0.2225(2) 0.21512(17) 0.0256(3) Uani 1 1 d . . . . .
C10 C 0.4599(3) -0.1074(2) 0.1985(2) 0.0384(5) Uani 1 1 d . . . . .
C11 C 0.5115(7) -0.0120(6) 0.1517(6) 0.107(2) Uani 1 1 d . . . . .
H11A H 0.5417 0.0727 0.2046 0.161 Uiso 1 1 calc R U . . .
H11B H 0.4315 -0.0082 0.0876 0.161 Uiso 1 1 calc R U . . .
H11C H 0.5949 -0.0382 0.1323 0.161 Uiso 1 1 calc R U . . .
C12 C 0.5862(5) -0.1195(5) 0.2942(4) 0.0826(15) Uani 1 1 d . . . . .
H12A H 0.6665 -0.1473 0.2713 0.124 Uiso 1 1 calc R U . . .
H12B H 0.5524 -0.1828 0.3240 0.124 Uiso 1 1 calc R U . . .
H12C H 0.6210 -0.0362 0.3491 0.124 Uiso 1 1 calc R U . . .
C13 C 0.3971(5) -0.2370(5) 0.1204(4) 0.0899(18) Uani 1 1 d . . . . .
H13A H 0.4764 -0.2797 0.1063 0.135 Uiso 1 1 calc R U . . .
H13B H 0.3281 -0.2282 0.0533 0.135 Uiso 1 1 calc R U . . .
H13C H 0.3454 -0.2883 0.1503 0.135 Uiso 1 1 calc R U . . .
C20 C 0.6539(2) 0.3337(2) 0.53167(17) 0.0265(4) Uani 1 1 d . . . . .
C21 C 0.6744(4) 0.4379(3) 0.6333(3) 0.0523(8) Uani 1 1 d . . . . .
H21A H 0.7784 0.4758 0.6691 0.078 Uiso 1 1 calc R U . . .
H21B H 0.6419 0.4010 0.6811 0.078 Uiso 1 1 calc R U . . .
H21C H 0.6163 0.5044 0.6154 0.078 Uiso 1 1 calc R U . . .
C22 C 0.7072(4) 0.3927(4) 0.4592(3) 0.0573(9) Uani 1 1 d . . . . .
H22A H 0.6545 0.4636 0.4455 0.086 Uiso 1 1 calc R U . . .
H22B H 0.6888 0.3274 0.3911 0.086 Uiso 1 1 calc R U . . .
H22C H 0.8127 0.4251 0.4943 0.086 Uiso 1 1 calc R U . . .
C23 C 0.7319(4) 0.2237(3) 0.5527(4) 0.0653(11) Uani 1 1 d . . . . .
H23A H 0.8378 0.2543 0.5874 0.098 Uiso 1 1 calc R U . . .
H23B H 0.7121 0.1578 0.4847 0.098 Uiso 1 1 calc R U . . .
H23C H 0.6969 0.1871 0.5996 0.098 Uiso 1 1 calc R U . . .
C30 C 0.1687(3) 0.2970(2) 0.04710(17) 0.0304(4) Uani 1 1 d . . . . .
C31 C 0.0098(3) 0.2493(4) -0.0258(3) 0.0530(8) Uani 1 1 d . . . . .
H31A H -0.0542 0.2904 0.0093 0.079 Uiso 1 1 calc R U . . .
H31B H -0.0117 0.1561 -0.0405 0.079 Uiso 1 1 calc R U . . .
H31C H -0.0075 0.2704 -0.0933 0.079 Uiso 1 1 calc R U . . .
C32 C 0.2047(4) 0.4422(3) 0.0750(2) 0.0420(6) Uani 1 1 d . . . . .
H32A H 0.1353 0.4819 0.1051 0.063 Uiso 1 1 calc R U . . .
H32B H 0.1973 0.4666 0.0101 0.063 Uiso 1 1 calc R U . . .
H32C H 0.3047 0.4717 0.1277 0.063 Uiso 1 1 calc R U . . .
C33 C 0.2721(3) 0.2322(3) -0.0023(2) 0.0427(6) Uani 1 1 d . . . . .
H33A H 0.2604 0.2533 -0.0692 0.064 Uiso 1 1 calc R U . . .
H33B H 0.2490 0.1391 -0.0175 0.064 Uiso 1 1 calc R U . . .
H33C H 0.3736 0.2623 0.0477 0.064 Uiso 1 1 calc R U . . .
N1 N 0.3477(3) -0.0563(2) 0.2355(2) 0.0385(5) Uani 1 1 d . . . . .
N2 N 0.4985(2) 0.2849(2) 0.47595(17) 0.0327(4) Uani 1 1 d . . . . .
N3 N 0.1901(2) 0.2636(2) 0.14574(17) 0.0335(4) Uani 1 1 d . . . . .
F1 F 0.6082(3) -0.4564(3) 0.2592(2) 0.0655(7) Uani 0.9 1 d . . P B 1
F2 F 0.6079(2) -0.5004(3) 0.10015(17) 0.0620(6) Uani 0.9 1 d . . P B 1
F3 F 0.6569(3) -0.6369(2) 0.1898(2) 0.0713(8) Uani 0.9 1 d . . P B 1
S1 S 0.86513(9) -0.44520(7) 0.24995(5) 0.02626(12) Uani 0.9 1 d . . P B 1
O1 O 0.9214(2) -0.4652(2) 0.35522(15) 0.0364(4) Uani 0.9 1 d . . P B 1
O2 O 0.8658(3) -0.3137(2) 0.2481(2) 0.0581(7) Uani 0.9 1 d . . P B 1
O3 O 0.9220(3) -0.5212(4) 0.1755(2) 0.0655(8) Uani 0.9 1 d . . P B 1
C40 C 0.6756(3) -0.5125(3) 0.1971(3) 0.0390(6) Uani 0.9 1 d . . P B 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C7 1.979(2) . ?
Re1 C8 1.992(2) . ?
Re1 C9 1.995(2) . ?
Re1 C2 2.235(2) . ?
Re1 C6 2.242(2) . ?
Re1 C4 2.257(2) . ?
Re1 C1 2.258(3) . ?
Re1 C3 2.267(3) . ?
Re1 C5 2.281(2) . ?
C1 C2 1.396(6) . ?
C1 C6 1.413(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.394(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.373(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 N1 1.166(3) . ?
C8 N2 1.166(3) . ?
C9 N3 1.156(3) . ?
C10 N1 1.446(3) . ?
C10 C13 1.491(5) . ?
C10 C11 1.499(5) . ?
C10 C12 1.522(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C20 N2 1.450(3) . ?
C20 C23 1.501(4) . ?
C20 C21 1.513(4) . ?
C20 C22 1.525(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C30 N3 1.452(3) . ?
C30 C31 1.516(4) . ?
C30 C33 1.518(4) . ?
C30 C32 1.522(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
F1 C40 1.310(4) . ?
F2 C40 1.326(3) . ?
F3 C40 1.333(4) . ?
S1 O3 1.440(3) . ?
S1 O2 1.442(3) . ?
S1 O1 1.4522(19) . ?
S1 C40 1.781(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Re1 C8 82.94(9) . . ?
C7 Re1 C9 84.39(9) . . ?
C8 Re1 C9 89.05(9) . . ?
C7 Re1 C2 93.19(10) . . ?
C8 Re1 C2 141.10(15) . . ?
C9 Re1 C2 129.25(15) . . ?
C7 Re1 C6 143.47(12) . . ?
C8 Re1 C6 132.51(12) . . ?
C9 Re1 C6 87.36(10) . . ?
C2 Re1 C6 65.39(13) . . ?
C7 Re1 C4 134.24(11) . . ?
C8 Re1 C4 91.12(10) . . ?
C9 Re1 C4 141.07(11) . . ?
C2 Re1 C4 64.28(13) . . ?
C6 Re1 C4 64.49(11) . . ?
C7 Re1 C1 109.67(11) . . ?
C8 Re1 C1 166.17(10) . . ?
C9 Re1 C1 97.64(12) . . ?
C2 Re1 C1 36.19(16) . . ?
C6 Re1 C1 36.61(13) . . ?
C4 Re1 C1 76.05(11) . . ?
C7 Re1 C3 104.08(10) . . ?
C8 Re1 C3 107.44(12) . . ?
C9 Re1 C3 162.11(11) . . ?
C2 Re1 C3 36.07(16) . . ?
C6 Re1 C3 76.45(11) . . ?
C4 Re1 C3 35.34(13) . . ?
C1 Re1 C3 64.78(14) . . ?
C7 Re1 C5 168.17(10) . . ?
C8 Re1 C5 101.82(10) . . ?
C9 Re1 C5 106.36(10) . . ?
C2 Re1 C5 76.27(10) . . ?
C6 Re1 C5 35.69(13) . . ?
C4 Re1 C5 35.89(12) . . ?
C1 Re1 C5 64.71(12) . . ?
C3 Re1 C5 64.23(11) . . ?
C2 C1 C6 118.8(3) . . ?
C2 C1 Re1 71.02(16) . . ?
C6 C1 Re1 71.06(15) . . ?
C2 C1 H1 120.6 . . ?
C6 C1 H1 120.6 . . ?
Re1 C1 H1 129.7 . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 Re1 73.21(16) . . ?
C1 C2 Re1 72.80(16) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
Re1 C2 H2 126.2 . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 Re1 71.92(15) . . ?
C2 C3 Re1 70.72(16) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
Re1 C3 H3 129.4 . . ?
C3 C4 C5 121.5(3) . . ?
C3 C4 Re1 72.74(16) . . ?
C5 C4 Re1 72.98(15) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
Re1 C4 H4 127.1 . . ?
C6 C5 C4 119.1(3) . . ?
C6 C5 Re1 70.62(15) . . ?
C4 C5 Re1 71.13(14) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
Re1 C5 H5 130.3 . . ?
C5 C6 C1 120.4(3) . . ?
C5 C6 Re1 73.68(15) . . ?
C1 C6 Re1 72.33(15) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
Re1 C6 H6 126.0 . . ?
N1 C7 Re1 176.7(2) . . ?
N2 C8 Re1 178.0(2) . . ?
N3 C9 Re1 176.1(2) . . ?
N1 C10 C13 109.0(3) . . ?
N1 C10 C11 106.6(3) . . ?
C13 C10 C11 113.7(4) . . ?
N1 C10 C12 108.6(3) . . ?
C13 C10 C12 109.2(3) . . ?
C11 C10 C12 109.7(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C20 C23 108.4(2) . . ?
N2 C20 C21 108.7(2) . . ?
C23 C20 C21 112.8(3) . . ?
N2 C20 C22 107.7(2) . . ?
C23 C20 C22 110.4(3) . . ?
C21 C20 C22 108.6(3) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C30 C31 107.8(2) . . ?
N3 C30 C33 107.6(2) . . ?
C31 C30 C33 111.3(2) . . ?
N3 C30 C32 108.1(2) . . ?
C31 C30 C32 111.0(2) . . ?
C33 C30 C32 110.9(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C7 N1 C10 161.5(3) . . ?
C8 N2 C20 171.6(2) . . ?
C9 N3 C30 169.9(3) . . ?
O3 S1 O2 113.8(2) . . ?
O3 S1 O1 112.78(16) . . ?
O2 S1 O1 116.07(16) . . ?
O3 S1 C40 103.27(18) . . ?
O2 S1 C40 104.29(16) . . ?
O1 S1 C40 104.85(14) . . ?
F1 C40 F2 107.8(3) . . ?
F1 C40 F3 106.9(3) . . ?
F2 C40 F3 107.7(3) . . ?
F1 C40 S1 110.9(2) . . ?
F2 C40 S1 111.9(2) . . ?
F3 C40 S1 111.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 3.2(4) . . . . ?
Re1 C1 C2 C3 57.6(2) . . . . ?
C6 C1 C2 Re1 -54.5(2) . . . . ?
C1 C2 C3 C4 -2.5(4) . . . . ?
Re1 C2 C3 C4 54.9(2) . . . . ?
C1 C2 C3 Re1 -57.4(2) . . . . ?
C2 C3 C4 C5 2.3(4) . . . . ?
Re1 C3 C4 C5 56.7(2) . . . . ?
C2 C3 C4 Re1 -54.3(2) . . . . ?
C3 C4 C5 C6 -2.8(4) . . . . ?
Re1 C4 C5 C6 53.8(2) . . . . ?
C3 C4 C5 Re1 -56.6(2) . . . . ?
C4 C5 C6 C1 3.5(4) . . . . ?
Re1 C5 C6 C1 57.4(2) . . . . ?
C4 C5 C6 Re1 -54.0(2) . . . . ?
C2 C1 C6 C5 -3.7(4) . . . . ?
Re1 C1 C6 C5 -58.1(2) . . . . ?
C2 C1 C6 Re1 54.4(2) . . . . ?
C13 C10 N1 C7 -155.2(9) . . . . ?
C11 C10 N1 C7 -32.2(10) . . . . ?
C12 C10 N1 C7 85.9(9) . . . . ?
C31 C30 N3 C9 26.2(15) . . . . ?
C33 C30 N3 C9 -94.0(14) . . . . ?
C32 C30 N3 C9 146.2(13) . . . . ?
O3 S1 C40 F1 177.4(2) . . . . ?
O2 S1 C40 F1 -63.4(3) . . . . ?
O1 S1 C40 F1 59.1(3) . . . . ?
O3 S1 C40 F2 -62.2(3) . . . . ?
O2 S1 C40 F2 57.0(3) . . . . ?
O1 S1 C40 F2 179.5(2) . . . . ?
O3 S1 C40 F3 58.4(3) . . . . ?
O2 S1 C40 F3 177.6(3) . . . . ?
O1 S1 C40 F3 -59.9(3) . . . . ?

_refine_diff_density_max         1.550
_refine_diff_density_min         -1.758
_refine_diff_density_rms         0.129

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_hb300517_twin1_hklf5
_database_code_depnum_ccdc_archive 'CCDC 1554160'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;

_refine_special_details          
;
Refined as a 2-component perfect twin: analysis of the reflections
with the CrysalisPro software (Rigaku OD, 2015) revealed that the
selected crystal consists of two components. The twin law corresponds
to a rotation of the two components around the a* axis with a twin
ratio of about 70:30. The final SHELXL refinements were done on a
HKLF5 file containing all component data including overlapped reflections.
;

_audit_creation_date             2017-05-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        'to be completed'
_chemical_formula_moiety         'C18 H25 N Tc, F6 P'
_chemical_formula_sum            'C18 H25 F6 N P Tc'
_chemical_formula_weight         498.36
_chemical_absolute_configuration ad
_chemical_melting_point          ?

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'
N N 0.0061 0.0033 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   8.1171(4)
_cell_length_b                   15.7539(7)
_cell_length_c                   15.0788(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.370(4)
_cell_angle_gamma                90
_cell_volume                     1927.67(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13209
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      2.5

_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.13a (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 -2 0.0205
1 -1 2 0.0205
0 1 0 0.0693
0 -1 0 0.0998
2 -2 1 0.0323
-2 2 -1 0.0208
-1 1 2 0.0175
1 -1 -2 0.0495
-2 1 -4 0.0214
-1 -3 -2 0.0865
-1 -2 2 0.0895
0 1 1 0.0451

_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21006
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.401
_diffrn_reflns_theta_min         2.586
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      183(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  78.00   0.50   60.00    --    4.71  77.00 -60.00  192
  2  ω     47.00  77.00   0.50   60.00    --    4.71  57.00-120.00   60
  3  ω     21.00  57.00   0.50   60.00    --   -5.80  57.00 -30.00   72
  4  ω     -7.00  82.00   0.50   60.00    --    4.71  38.00 -30.00  178
  5  ω     -1.00  82.00   0.50   60.00    --    4.71  38.00 120.00  166
  6  ω    -25.00  19.00   0.50   60.00    --   -5.80 -99.00  90.00   88
  7  ω     44.00  82.00   0.50   60.00    --    4.71-169.00 128.00   76
  8  ω    -68.00  20.00   0.50   60.00    --    4.71 -57.00 -90.00  176
  9  ω     -9.00  36.00   0.50   60.00    --    4.71  57.00-120.00   90
 10  ω     38.00  84.00   0.50   60.00    --    4.71 178.00-180.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0400644000
_diffrn_orient_matrix_UB_12      -0.0325304000
_diffrn_orient_matrix_UB_13      0.0237757000
_diffrn_orient_matrix_UB_21      -0.0253260000
_diffrn_orient_matrix_UB_22      0.0302432000
_diffrn_orient_matrix_UB_23      0.0317558000
_diffrn_orient_matrix_UB_31      -0.0734474000
_diffrn_orient_matrix_UB_32      0.0073652000
_diffrn_orient_matrix_UB_33      -0.0253035000

_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                20410
_reflns_number_total             21006

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         21006
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0498
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1125P)²+0.3289P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1356

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
2.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.0814(18) 0.4882(7) 0.4396(5) 0.083(4) Uani 1 1 d . . . . .
F2 F 0.3044(16) 0.4852(9) 0.3572(12) 0.102(5) Uani 1 1 d . . . . .
F3 F 0.0893(16) 0.4099(6) 0.3146(5) 0.076(3) Uani 1 1 d . . . . .
F4 F 0.154(2) 0.5265(7) 0.2374(6) 0.108(5) Uani 1 1 d . . . . .
F5 F -0.0724(17) 0.5303(14) 0.3261(9) 0.115(5) Uani 1 1 d . . . . .
F6 F 0.1499(15) 0.6049(5) 0.3613(6) 0.074(3) Uani 1 1 d . . . . .
P1 P 0.1167(4) 0.5076(2) 0.33806(16) 0.0391(6) Uani 1 1 d . . . . .
C1 C 0.4254(14) 0.7419(8) 0.6019(8) 0.036(2) Uani 1 1 d . . . . .
C2 C 0.4874(14) 0.6776(8) 0.6634(6) 0.037(2) Uani 1 1 d . . . . .
C3 C 0.5579(13) 0.6021(7) 0.6292(6) 0.034(2) Uani 1 1 d . . . . .
C4 C 0.5789(13) 0.5917(6) 0.5363(6) 0.0310(19) Uani 1 1 d . . . . .
C5 C 0.5278(13) 0.6571(6) 0.4769(5) 0.032(2) Uani 1 1 d . . . . .
C6 C 0.4416(19) 0.7283(8) 0.5101(10) 0.032(3) Uani 1 1 d . . . . .
C7 C 0.3445(18) 0.8219(10) 0.6357(10) 0.054(3) Uani 1 1 d . . . . .
H7A H 0.384481 0.871000 0.602630 0.082 Uiso 1 1 calc GR . . . .
H7B H 0.371893 0.829115 0.698920 0.082 Uiso 1 1 calc GR . . . .
H7C H 0.224673 0.817339 0.627488 0.082 Uiso 1 1 calc GR . . . .
C8 C 0.467(2) 0.6915(10) 0.7621(7) 0.058(4) Uani 1 1 d . . . . .
H8A H 0.524422 0.646408 0.795221 0.087 Uiso 1 1 calc GR . . . .
H8B H 0.349555 0.690401 0.775786 0.087 Uiso 1 1 calc GR . . . .
H8C H 0.513718 0.746681 0.779101 0.087 Uiso 1 1 calc GR . . . .
C9 C 0.617(2) 0.5322(9) 0.6920(8) 0.055(3) Uani 1 1 d . . . . .
H9A H 0.640755 0.556321 0.750885 0.083 Uiso 1 1 calc GR . . . .
H9B H 0.717836 0.506513 0.669202 0.083 Uiso 1 1 calc GR . . . .
H9C H 0.531664 0.488631 0.696416 0.083 Uiso 1 1 calc GR . . . .
C10 C 0.6552(17) 0.5110(8) 0.5012(8) 0.048(3) Uani 1 1 d . . . . .
H10A H 0.583105 0.462776 0.513596 0.072 Uiso 1 1 calc GR . . . .
H10B H 0.763028 0.502040 0.530250 0.072 Uiso 1 1 calc GR . . . .
H10C H 0.668710 0.516098 0.436994 0.072 Uiso 1 1 calc GR . . . .
C11 C 0.5639(17) 0.6494(9) 0.3791(6) 0.049(3) Uani 1 1 d . . . . .
H11A H 0.467380 0.625831 0.347522 0.074 Uiso 1 1 calc GR . . . .
H11B H 0.658533 0.611691 0.371505 0.074 Uiso 1 1 calc GR . . . .
H11C H 0.589002 0.705588 0.355121 0.074 Uiso 1 1 calc GR . . . .
C12 C 0.365(2) 0.7925(9) 0.4454(10) 0.052(3) Uani 1 1 d . . . . .
H12A H 0.249508 0.777132 0.432870 0.079 Uiso 1 1 calc GR . . . .
H12B H 0.425660 0.792136 0.390064 0.079 Uiso 1 1 calc GR . . . .
H12C H 0.369750 0.849274 0.471776 0.079 Uiso 1 1 calc GR . . . .
C13 C 0.9754(12) 0.6855(7) 0.5885(6) 0.0329(18) Uani 1 1 d . . . . .
C14 C 0.9298(17) 0.7262(8) 0.5066(8) 0.036(3) Uani 1 1 d . . . . .
H14 H 0.952345 0.698381 0.452330 0.043 Uiso 1 1 calc R . . . .
C15 C 0.8530(16) 0.8055(8) 0.5041(6) 0.038(2) Uani 1 1 d . . . . .
H15 H 0.829802 0.832159 0.448686 0.045 Uiso 1 1 calc R . . . .
C16 C 0.8098(13) 0.8464(6) 0.5836(7) 0.0367(19) Uani 1 1 d . . . . .
H16 H 0.760786 0.901161 0.582326 0.044 Uiso 1 1 calc R . . . .
C17 C 0.8411(14) 0.8038(8) 0.6658(6) 0.035(2) Uani 1 1 d . . . . .
H17 H 0.810476 0.829977 0.719732 0.042 Uiso 1 1 calc R . . . .
C18 C 0.916(2) 0.7238(8) 0.6676(9) 0.034(3) Uani 1 1 d . . . . .
H18 H 0.928711 0.694503 0.722467 0.041 Uiso 1 1 calc R . . . .
N1 N 1.0634(15) 0.6134(7) 0.5917(7) 0.052(2) Uani 1 1 d . . . . .
H1A H 1.085548 0.588942 0.643119 0.062 Uiso 1 1 calc R . . . .
H1B H 1.098838 0.590500 0.542474 0.062 Uiso 1 1 calc R . . . .
Tc1 Tc 0.69428(8) 0.71725(3) 0.57832(6) 0.0235(3) 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
F1 P1 1.594(8) . ?
F2 P1 1.583(13) . ?
F3 P1 1.593(9) . ?
F4 P1 1.583(7) . ?
F5 P1 1.583(14) . ?
F6 P1 1.595(9) . ?
C1 C2 1.455(17) . ?
C1 C6 1.41(2) . ?
C1 C7 1.515(17) . ?
C1 Tc1 2.253(11) . ?
C2 C3 1.422(17) . ?
C2 C8 1.517(14) . ?
C2 Tc1 2.227(10) . ?
C3 C4 1.425(13) . ?
C3 C9 1.525(13) . ?
C3 Tc1 2.268(10) . ?
C4 C5 1.421(14) . ?
C4 C10 1.514(14) . ?
C4 Tc1 2.273(9) . ?
C5 C6 1.418(19) . ?
C5 C11 1.515(13) . ?
C5 Tc1 2.227(8) . ?
C6 C12 1.528(18) . ?
C6 Tc1 2.279(16) . ?
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 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.432(16) . ?
C13 C18 1.431(17) . ?
C13 N1 1.342(16) . ?
C13 Tc1 2.338(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.40(2) . ?
C14 Tc1 2.223(13) . ?
C15 H15 0.9500 . ?
C15 C16 1.412(16) . ?
C15 Tc1 2.217(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.427(15) . ?
C16 Tc1 2.241(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.402(19) . ?
C17 Tc1 2.224(10) . ?
C18 H18 0.9500 . ?
C18 Tc1 2.228(15) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?

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
F1 P1 F6 90.3(5) . . ?
F2 P1 F1 88.7(9) . . ?
F2 P1 F3 87.4(7) . . ?
F2 P1 F6 91.0(7) . . ?
F3 P1 F1 90.1(5) . . ?
F3 P1 F6 178.3(7) . . ?
F4 P1 F1 179.3(9) . . ?
F4 P1 F2 90.6(10) . . ?
F4 P1 F3 89.9(5) . . ?
F4 P1 F5 93.2(9) . . ?
F4 P1 F6 89.7(5) . . ?
F5 P1 F1 87.5(8) . . ?
F5 P1 F2 176.1(9) . . ?
F5 P1 F3 93.6(9) . . ?
F5 P1 F6 88.0(9) . . ?
C2 C1 C7 120.7(11) . . ?
C2 C1 Tc1 70.1(6) . . ?
C6 C1 C2 118.7(11) . . ?
C6 C1 C7 120.6(11) . . ?
C6 C1 Tc1 72.9(8) . . ?
C7 C1 Tc1 128.8(9) . . ?
C1 C2 C8 118.8(12) . . ?
C1 C2 Tc1 72.0(6) . . ?
C3 C2 C1 119.1(8) . . ?
C3 C2 C8 122.1(11) . . ?
C3 C2 Tc1 73.1(6) . . ?
C8 C2 Tc1 128.8(9) . . ?
C2 C3 C4 120.8(9) . . ?
C2 C3 C9 120.2(9) . . ?
C2 C3 Tc1 70.0(6) . . ?
C4 C3 C9 118.9(10) . . ?
C4 C3 Tc1 71.9(6) . . ?
C9 C3 Tc1 129.7(8) . . ?
C3 C4 C10 120.0(9) . . ?
C3 C4 Tc1 71.5(6) . . ?
C5 C4 C3 119.7(9) . . ?
C5 C4 C10 120.3(9) . . ?
C5 C4 Tc1 69.9(5) . . ?
C10 C4 Tc1 131.2(8) . . ?
C4 C5 C11 119.6(10) . . ?
C4 C5 Tc1 73.3(5) . . ?
C6 C5 C4 119.4(9) . . ?
C6 C5 C11 121.0(10) . . ?
C6 C5 Tc1 73.7(7) . . ?
C11 C5 Tc1 125.0(7) . . ?
C1 C6 C5 121.6(12) . . ?
C1 C6 C12 118.6(14) . . ?
C1 C6 Tc1 70.9(8) . . ?
C5 C6 C12 119.7(13) . . ?
C5 C6 Tc1 69.7(7) . . ?
C12 C6 Tc1 133.5(10) . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C9 H9A 109.5 . . ?
C3 C9 H9B 109.5 . . ?
C3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C5 C11 H11A 109.5 . . ?
C5 C11 H11B 109.5 . . ?
C5 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C6 C12 H12A 109.5 . . ?
C6 C12 H12B 109.5 . . ?
C6 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 Tc1 67.4(7) . . ?
C18 C13 C14 116.5(10) . . ?
C18 C13 Tc1 67.6(8) . . ?
N1 C13 C14 122.5(9) . . ?
N1 C13 C18 121.0(9) . . ?
N1 C13 Tc1 134.5(8) . . ?
C13 C14 H14 119.0 . . ?
C13 C14 Tc1 76.1(6) . . ?
C15 C14 C13 122.0(10) . . ?
C15 C14 H14 119.0 . . ?
C15 C14 Tc1 71.4(7) . . ?
Tc1 C14 H14 125.1 . . ?
C14 C15 H15 119.8 . . ?
C14 C15 C16 120.3(9) . . ?
C14 C15 Tc1 71.9(7) . . ?
C16 C15 H15 119.8 . . ?
C16 C15 Tc1 72.4(5) . . ?
Tc1 C15 H15 128.0 . . ?
C15 C16 H16 120.6 . . ?
C15 C16 C17 118.7(10) . . ?
C15 C16 Tc1 70.6(6) . . ?
C17 C16 H16 120.6 . . ?
C17 C16 Tc1 70.7(6) . . ?
Tc1 C16 H16 130.5 . . ?
C16 C17 H17 119.7 . . ?
C16 C17 Tc1 72.0(5) . . ?
C18 C17 C16 120.6(9) . . ?
C18 C17 H17 119.7 . . ?
C18 C17 Tc1 71.8(7) . . ?
Tc1 C17 H17 128.8 . . ?
C13 C18 H18 119.4 . . ?
C13 C18 Tc1 76.0(7) . . ?
C17 C18 C13 121.2(10) . . ?
C17 C18 H18 119.4 . . ?
C17 C18 Tc1 71.5(8) . . ?
Tc1 C18 H18 124.7 . . ?
C13 N1 H1A 120.0 . . ?
C13 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C1 Tc1 C3 66.6(4) . . ?
C1 Tc1 C4 78.5(4) . . ?
C1 Tc1 C6 36.3(5) . . ?
C1 Tc1 C13 167.0(4) . . ?
C2 Tc1 C1 37.9(4) . . ?
C2 Tc1 C3 36.9(4) . . ?
C2 Tc1 C4 66.8(4) . . ?
C2 Tc1 C6 66.3(5) . . ?
C2 Tc1 C13 130.6(4) . . ?
C2 Tc1 C16 123.7(4) . . ?
C2 Tc1 C18 106.0(5) . . ?
C3 Tc1 C4 36.6(3) . . ?
C3 Tc1 C6 76.8(4) . . ?
C3 Tc1 C13 106.9(4) . . ?
C4 Tc1 C6 65.2(4) . . ?
C4 Tc1 C13 103.1(4) . . ?
C5 Tc1 C1 66.9(4) . . ?
C5 Tc1 C2 79.8(4) . . ?
C5 Tc1 C3 66.4(3) . . ?
C5 Tc1 C4 36.8(4) . . ?
C5 Tc1 C6 36.7(5) . . ?
C5 Tc1 C13 121.9(4) . . ?
C5 Tc1 C16 131.1(4) . . ?
C5 Tc1 C18 154.7(4) . . ?
C6 Tc1 C13 155.8(5) . . ?
C14 Tc1 C1 155.9(4) . . ?
C14 Tc1 C2 165.3(5) . . ?
C14 Tc1 C3 130.4(4) . . ?
C14 Tc1 C4 105.8(4) . . ?
C14 Tc1 C5 102.0(4) . . ?
C14 Tc1 C6 123.4(5) . . ?
C14 Tc1 C13 36.5(4) . . ?
C14 Tc1 C16 66.2(4) . . ?
C14 Tc1 C17 78.2(4) . . ?
C14 Tc1 C18 66.3(5) . . ?
C15 Tc1 C1 123.2(5) . . ?
C15 Tc1 C2 157.2(5) . . ?
C15 Tc1 C3 165.2(4) . . ?
C15 Tc1 C4 130.2(4) . . ?
C15 Tc1 C5 105.7(4) . . ?
C15 Tc1 C6 104.6(4) . . ?
C15 Tc1 C13 65.7(4) . . ?
C15 Tc1 C14 36.7(5) . . ?
C15 Tc1 C16 36.9(4) . . ?
C15 Tc1 C17 66.7(4) . . ?
C15 Tc1 C18 78.7(5) . . ?
C16 Tc1 C1 104.1(4) . . ?
C16 Tc1 C3 157.1(4) . . ?
C16 Tc1 C4 165.8(3) . . ?
C16 Tc1 C6 108.6(4) . . ?
C16 Tc1 C13 77.6(4) . . ?
C17 Tc1 C1 107.9(4) . . ?
C17 Tc1 C2 103.3(4) . . ?
C17 Tc1 C3 123.3(4) . . ?
C17 Tc1 C4 155.6(4) . . ?
C17 Tc1 C5 167.3(4) . . ?
C17 Tc1 C6 133.2(5) . . ?
C17 Tc1 C13 65.4(4) . . ?
C17 Tc1 C16 37.3(4) . . ?
C17 Tc1 C18 36.7(5) . . ?
C18 Tc1 C1 132.1(5) . . ?
C18 Tc1 C3 103.1(4) . . ?
C18 Tc1 C4 122.1(4) . . ?
C18 Tc1 C6 167.5(4) . . ?
C18 Tc1 C13 36.4(5) . . ?
C18 Tc1 C16 66.7(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A F4 0.88 2.37 3.186(16) 154.9 2_665
N1 H1B F1 0.88 2.24 3.031(13) 149.6 1_655



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_GIM040716
_database_code_depnum_ccdc_archive 'CCDC 1554403'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H54 F9 Li2 N6 O11 Re S3'
_chemical_formula_weight         1178.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.191(2)
_cell_length_b                   17.740(3)
_cell_length_c                   17.909(4)
_cell_angle_alpha                117.46(2)
_cell_angle_beta                 102.485(19)
_cell_angle_gamma                93.314(16)
_cell_volume                     2758.0(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    15480
_cell_measurement_theta_min      2.6060
_cell_measurement_theta_max      32.1330

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    2.397
_shelx_estimated_absorpt_T_min   0.358
_shelx_estimated_absorpt_T_max   0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.56980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Oxford Xcalibur Ruby CCD'
_diffrn_measurement_method       'ο oscillation scan'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_reflns_number            40102
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.251
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_full        30.44
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             16824
_reflns_number_gt                13188
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro (Oxford, 2007)'
_computing_cell_refinement       'CrysAlisPro (Oxford, 2007)'
_computing_data_reduction        'CrysAlisPro (Oxford, 2007)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0507P)²+1.3483P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16824
_refine_ls_number_parameters     604
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1114
_refine_ls_wR_factor_gt          0.1002
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re -0.00114(2) 0.13042(2) -0.21004(2) 0.04951(6) Uani 1 1 d . . . . .
C1 C -0.1196(4) 0.0125(2) -0.2965(2) 0.0494(8) Uani 1 1 d . . . . .
C2 C -0.0792(3) 0.19019(19) -0.2794(2) 0.0437(7) Uani 1 1 d . . . . .
C3 C 0.1410(5) 0.0934(2) -0.2781(3) 0.0581(9) Uani 1 1 d . . . . .
C4 C 0.1213(4) 0.2459(2) -0.1176(2) 0.0494(8) Uani 1 1 d . . . . .
C5 C 0.0830(4) 0.0798(2) -0.1346(2) 0.0548(9) Uani 1 1 d . . . . .
C6 C -0.1467(4) 0.1682(2) -0.1447(2) 0.0539(9) Uani 1 1 d . . . . .
C7 C -0.2289(4) -0.1487(2) -0.3861(3) 0.0612(10) Uani 1 1 d . . . . .
C8 C -0.1308(8) -0.1924(4) -0.4363(7) 0.161(4) Uani 1 1 d . . . . .
H8A H -0.1219 -0.1702 -0.4762 0.241 Uiso 1 1 calc R U . . .
H8B H -0.1650 -0.2549 -0.4700 0.241 Uiso 1 1 calc R U . . .
H8C H -0.0413 -0.1809 -0.3954 0.241 Uiso 1 1 calc R U . . .
C9 C -0.3651(6) -0.1709(4) -0.4499(4) 0.109(2) Uani 1 1 d . . . . .
H9A H -0.3946 -0.2338 -0.4827 0.163 Uiso 1 1 calc R U . . .
H9B H -0.3584 -0.1492 -0.4905 0.163 Uiso 1 1 calc R U . . .
H9C H -0.4318 -0.1444 -0.4183 0.163 Uiso 1 1 calc R U . . .
C10 C -0.2419(13) -0.1715(5) -0.3174(5) 0.191(5) Uani 1 1 d . . . . .
H10A H -0.1507 -0.1660 -0.2814 0.286 Uiso 1 1 calc R U . . .
H10B H -0.2906 -0.2312 -0.3452 0.286 Uiso 1 1 calc R U . . .
H10C H -0.2930 -0.1324 -0.2803 0.286 Uiso 1 1 calc R U . . .
C11 C -0.1702(3) 0.2941(2) -0.3339(2) 0.0464(7) Uani 1 1 d . . . . .
C12 C -0.3239(5) 0.2735(5) -0.3607(6) 0.117(3) Uani 1 1 d . . . . .
H12A H -0.3606 0.3167 -0.3747 0.176 Uiso 1 1 calc R U . . .
H12B H -0.3558 0.2743 -0.3126 0.176 Uiso 1 1 calc R U . . .
H12C H -0.3553 0.2161 -0.4124 0.176 Uiso 1 1 calc R U . . .
C13 C -0.1124(7) 0.3809(3) -0.2533(3) 0.0831(15) Uani 1 1 d . . . . .
H13A H -0.1469 0.3835 -0.2053 0.125 Uiso 1 1 calc R U . . .
H13B H -0.1404 0.4267 -0.2659 0.125 Uiso 1 1 calc R U . . .
H13C H -0.0124 0.3888 -0.2365 0.125 Uiso 1 1 calc R U . . .
C14 C -0.1148(5) 0.2901(3) -0.4076(3) 0.0678(11) Uani 1 1 d . . . . .
H14C H -0.0150 0.3067 -0.3869 0.102 Uiso 1 1 calc R U . . .
H14B H -0.1533 0.3299 -0.4264 0.102 Uiso 1 1 calc R U . . .
H14A H -0.1403 0.2311 -0.4569 0.102 Uiso 1 1 calc R U . . .
C15 C 0.2892(6) 0.0181(3) -0.3802(3) 0.0839(15) Uani 1 1 d . . . . .
C16 C 0.3159(8) -0.0563(4) -0.3639(5) 0.121(2) Uani 1 1 d . . . . .
H16A H 0.3495 -0.0986 -0.4109 0.181 Uiso 1 1 calc R U . . .
H16B H 0.2309 -0.0838 -0.3625 0.181 Uiso 1 1 calc R U . . .
H16C H 0.3846 -0.0350 -0.3076 0.181 Uiso 1 1 calc R U . . .
C17 C 0.1982(9) -0.0156(5) -0.4720(4) 0.133(3) Uani 1 1 d . . . . .
H17A H 0.1088 -0.0444 -0.4775 0.199 Uiso 1 1 calc R U . . .
H17B H 0.2404 -0.0570 -0.5142 0.199 Uiso 1 1 calc R U . . .
H17C H 0.1864 0.0327 -0.4838 0.199 Uiso 1 1 calc R U . . .
C18 C 0.4202(9) 0.0742(6) -0.3656(6) 0.150(3) Uani 1 1 d . . . . .
H18A H 0.4631 0.0426 -0.4123 0.225 Uiso 1 1 calc R U . . .
H18B H 0.4828 0.0889 -0.3090 0.225 Uiso 1 1 calc R U . . .
H18C H 0.3994 0.1273 -0.3660 0.225 Uiso 1 1 calc R U . . .
C19 C 0.2567(4) 0.3882(2) 0.0158(2) 0.0610(10) Uani 1 1 d . . . . .
C20 C 0.3281(6) 0.3600(4) 0.0803(3) 0.105(2) Uani 1 1 d . . . . .
H20A H 0.2601 0.3264 0.0897 0.157 Uiso 1 1 calc R U . . .
H20B H 0.3758 0.4111 0.1360 0.157 Uiso 1 1 calc R U . . .
H20C H 0.3942 0.3243 0.0565 0.157 Uiso 1 1 calc R U . . .
C21 C 0.1549(9) 0.4411(4) 0.0493(6) 0.161(4) Uani 1 1 d . . . . .
H21A H 0.2003 0.4919 0.1059 0.242 Uiso 1 1 calc R U . . .
H21B H 0.0849 0.4067 0.0566 0.242 Uiso 1 1 calc R U . . .
H21C H 0.1118 0.4597 0.0076 0.242 Uiso 1 1 calc R U . . .
C22 C 0.3617(5) 0.4360(4) -0.0041(3) 0.0811(14) Uani 1 1 d . . . . .
H22C H 0.3144 0.4574 -0.0421 0.122 Uiso 1 1 calc R U . . .
H22B H 0.4196 0.3964 -0.0337 0.122 Uiso 1 1 calc R U . . .
H22A H 0.4187 0.4847 0.0507 0.122 Uiso 1 1 calc R U . . .
C23 C 0.2275(6) 0.0213(4) -0.0447(4) 0.0914(16) Uani 1 1 d . . . . .
C24 C 0.1462(14) -0.0635(9) -0.0604(12) 0.289(10) Uani 1 1 d . . . . .
H24A H 0.1961 -0.0814 -0.0197 0.434 Uiso 1 1 calc R U . . .
H24B H 0.1347 -0.1088 -0.1207 0.434 Uiso 1 1 calc R U . . .
H24C H 0.0562 -0.0540 -0.0506 0.434 Uiso 1 1 calc R U . . .
C25 C 0.3301(10) -0.0118(8) -0.0931(7) 0.191(5) Uani 1 1 d . . . . .
H25A H 0.2840 -0.0475 -0.1557 0.287 Uiso 1 1 calc R U . . .
H25B H 0.3799 -0.0468 -0.0717 0.287 Uiso 1 1 calc R U . . .
H25C H 0.3944 0.0369 -0.0840 0.287 Uiso 1 1 calc R U . . .
C26 C 0.2804(14) 0.0833(8) 0.0425(5) 0.254(8) Uani 1 1 d . . . . .
H26A H 0.3298 0.0570 0.0750 0.380 Uiso 1 1 calc R U . . .
H26B H 0.2056 0.1066 0.0672 0.380 Uiso 1 1 calc R U . . .
H26C H 0.3433 0.1301 0.0471 0.380 Uiso 1 1 calc R U . . .
C27 C -0.3125(5) 0.2450(3) -0.0567(3) 0.0688(11) Uani 1 1 d . . . . .
C28 C -0.2771(9) 0.3361(5) -0.0387(7) 0.149(4) Uani 1 1 d . . . . .
H28A H -0.1817 0.3599 -0.0038 0.223 Uiso 1 1 calc R U . . .
H28B H -0.3370 0.3713 -0.0063 0.223 Uiso 1 1 calc R U . . .
H28C H -0.2894 0.3368 -0.0941 0.223 Uiso 1 1 calc R U . . .
C29 C -0.2877(12) 0.2468(8) 0.0271(5) 0.206(6) Uani 1 1 d . . . . .
H29A H -0.3395 0.2867 0.0628 0.308 Uiso 1 1 calc R U . . .
H29B H -0.1900 0.2661 0.0575 0.308 Uiso 1 1 calc R U . . .
H29C H -0.3170 0.1887 0.0176 0.308 Uiso 1 1 calc R U . . .
C30 C -0.4587(8) 0.2103(6) -0.1116(6) 0.162(4) Uani 1 1 d . . . . .
H30A H -0.4701 0.2164 -0.1642 0.243 Uiso 1 1 calc R U . . .
H30B H -0.5192 0.2428 -0.0777 0.243 Uiso 1 1 calc R U . . .
H30C H -0.4820 0.1492 -0.1287 0.243 Uiso 1 1 calc R U . . .
C40 C 0.1062(4) 0.3331(3) 0.2383(3) 0.0599(9) Uani 1 1 d . . . . .
C50 C -0.3473(5) 0.2598(3) 0.2769(3) 0.0777(13) Uani 1 1 d . . . . .
C60 C -0.3294(4) 0.6533(3) 0.2643(2) 0.0571(9) Uani 1 1 d . . . . .
N1 N -0.1796(4) -0.05641(18) -0.3432(2) 0.0592(8) Uani 1 1 d . . . . .
N2 N -0.1234(3) 0.22906(18) -0.31281(19) 0.0477(6) Uani 1 1 d . . . . .
N3 N 0.2186(5) 0.0693(2) -0.3183(3) 0.0746(10) Uani 1 1 d . . . . .
N4 N 0.1861(3) 0.31039(19) -0.06241(19) 0.0556(7) Uani 1 1 d . . . . .
N5 N 0.1335(4) 0.0519(2) -0.0905(2) 0.0708(10) Uani 1 1 d . . . . .
N6 N -0.2261(4) 0.1949(2) -0.1068(3) 0.0706(10) Uani 1 1 d . . . . .
O1 O 0.0658(2) 0.47879(18) 0.34753(18) 0.0568(6) Uani 1 1 d . . . . .
O2 O 0.2860(2) 0.47253(16) 0.31810(16) 0.0464(5) Uani 1 1 d . . . . .
O3 O 0.2241(2) 0.40793(17) 0.40296(15) 0.0481(5) Uani 1 1 d . . . . .
O4 O -0.4445(2) 0.39869(19) 0.3455(2) 0.0638(7) Uani 1 1 d . . . . .
O5 O -0.3226(4) 0.3506(2) 0.4401(2) 0.0794(9) Uani 1 1 d . . . . .
O6 O -0.2009(2) 0.40994(18) 0.3739(2) 0.0723(9) Uani 1 1 d . . . . .
O7 O -0.2102(2) 0.5570(2) 0.3159(2) 0.0679(8) Uani 1 1 d . . . . .
O8 O -0.3390(3) 0.4924(2) 0.16372(17) 0.0657(7) Uani 1 1 d . . . . .
O9 O -0.4556(2) 0.5329(2) 0.27646(17) 0.0587(7) Uani 1 1 d . . . . .
O10 O -0.4641(2) 0.58884(18) 0.47576(15) 0.0542(6) Uani 1 1 d . . . . .
O11 O -0.0377(2) 0.59752(16) 0.49994(14) 0.0452(5) Uani 1 1 d . . . . .
F1 F 0.0090(3) 0.28831(18) 0.24777(18) 0.0861(8) Uani 1 1 d . . . . .
F2 F 0.0519(3) 0.3464(2) 0.17200(17) 0.0986(10) Uani 1 1 d . . . . .
F3 F 0.2009(3) 0.28566(18) 0.21618(18) 0.0890(9) Uani 1 1 d . . . . .
F4 F -0.4599(4) 0.2102(2) 0.2641(3) 0.1361(15) Uani 1 1 d . . . . .
F5 F -0.3470(6) 0.2616(3) 0.2066(2) 0.1548(18) Uani 1 1 d . . . . .
F6 F -0.2416(4) 0.2227(2) 0.2928(3) 0.1201(13) Uani 1 1 d . . . . .
F7 F -0.3278(4) 0.7109(2) 0.34384(19) 0.1095(11) Uani 1 1 d . . . . .
F8 F -0.4412(3) 0.6548(2) 0.21127(19) 0.0857(8) Uani 1 1 d . . . . .
F9 F -0.2237(3) 0.6766(2) 0.2440(2) 0.0953(9) Uani 1 1 d . . . . .
S1 S 0.17898(6) 0.43374(5) 0.33727(5) 0.03491(14) Uani 1 1 d . . . . .
S2 S -0.32659(7) 0.36700(5) 0.36859(5) 0.03867(15) Uani 1 1 d . . . . .
S3 S -0.33396(7) 0.54624(6) 0.25311(5) 0.03860(16) Uani 1 1 d . . . . .
Li1 Li -0.0993(5) 0.5115(4) 0.3784(3) 0.0395(11) Uani 1 1 d . . . . .
Li2 Li -0.5151(5) 0.5007(4) 0.3543(3) 0.0397(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
Re1 C5 2.018(4) . ?
Re1 C1 2.036(4) . ?
Re1 C3 2.037(4) . ?
Re1 C6 2.040(4) . ?
Re1 C4 2.044(4) . ?
Re1 C2 2.046(3) . ?
C1 N1 1.147(5) . ?
C2 N2 1.155(4) . ?
C3 N3 1.153(5) . ?
C4 N4 1.144(4) . ?
C5 N5 1.161(5) . ?
C6 N6 1.151(5) . ?
C7 N1 1.450(4) . ?
C7 C10 1.489(8) . ?
C7 C9 1.491(7) . ?
C7 C8 1.498(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N2 1.445(4) . ?
C11 C12 1.504(6) . ?
C11 C13 1.509(6) . ?
C11 C14 1.519(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14C 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14A 0.9800 . ?
C15 N3 1.436(6) . ?
C15 C16 1.506(8) . ?
C15 C17 1.514(8) . ?
C15 C18 1.515(10) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
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 N4 1.432(4) . ?
C19 C21 1.477(7) . ?
C19 C20 1.524(7) . ?
C19 C22 1.526(6) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22C 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22A 0.9800 . ?
C23 C26 1.387(10) . ?
C23 N5 1.421(5) . ?
C23 C25 1.477(10) . ?
C23 C24 1.548(12) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 N6 1.438(6) . ?
C27 C29 1.453(8) . ?
C27 C28 1.499(9) . ?
C27 C30 1.506(9) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C40 F3 1.322(5) . ?
C40 F1 1.322(5) . ?
C40 F2 1.327(5) . ?
C40 S1 1.799(4) . ?
C50 F5 1.274(6) . ?
C50 F4 1.314(6) . ?
C50 F6 1.340(6) . ?
C50 S2 1.812(4) . ?
C60 F9 1.312(5) . ?
C60 F7 1.312(5) . ?
C60 F8 1.326(4) . ?
C60 S3 1.812(4) . ?
O1 S1 1.437(2) . ?
O1 Li1 1.922(5) . ?
O2 S1 1.440(2) . ?
O2 Li2 1.948(5) 1_655 ?
O3 S1 1.447(2) . ?
O4 S2 1.417(2) . ?
O4 Li2 1.938(6) . ?
O5 S2 1.432(3) . ?
O6 S2 1.413(3) . ?
O6 Li1 1.984(6) . ?
O7 S3 1.433(2) . ?
O7 Li1 1.891(5) . ?
O8 S3 1.424(3) . ?
O9 S3 1.431(2) . ?
O9 Li2 1.924(5) . ?
O10 Li2 1.930(6) . ?
O11 Li1 1.922(6) . ?
Li2 O2 1.948(5) 1_455 ?

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 Re1 C1 88.68(14) . . ?
C5 Re1 C3 89.96(16) . . ?
C1 Re1 C3 87.74(15) . . ?
C5 Re1 C6 91.71(15) . . ?
C1 Re1 C6 91.92(15) . . ?
C3 Re1 C6 178.28(14) . . ?
C5 Re1 C4 87.67(14) . . ?
C1 Re1 C4 176.26(12) . . ?
C3 Re1 C4 93.01(15) . . ?
C6 Re1 C4 87.44(15) . . ?
C5 Re1 C2 175.93(12) . . ?
C1 Re1 C2 95.36(13) . . ?
C3 Re1 C2 90.76(14) . . ?
C6 Re1 C2 87.60(14) . . ?
C4 Re1 C2 88.29(13) . . ?
N1 C1 Re1 175.4(3) . . ?
N2 C2 Re1 174.9(3) . . ?
N3 C3 Re1 177.5(4) . . ?
N4 C4 Re1 176.0(3) . . ?
N5 C5 Re1 178.8(4) . . ?
N6 C6 Re1 175.6(3) . . ?
N1 C7 C10 107.8(4) . . ?
N1 C7 C9 109.4(4) . . ?
C10 C7 C9 109.8(6) . . ?
N1 C7 C8 107.2(4) . . ?
C10 C7 C8 114.6(7) . . ?
C9 C7 C8 108.0(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 106.5(4) . . ?
N2 C11 C13 107.4(3) . . ?
C12 C11 C13 113.2(5) . . ?
N2 C11 C14 108.8(3) . . ?
C12 C11 C14 111.7(4) . . ?
C13 C11 C14 109.1(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14C 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14C C14 H14B 109.5 . . ?
C11 C14 H14A 109.5 . . ?
H14C C14 H14A 109.5 . . ?
H14B C14 H14A 109.5 . . ?
N3 C15 C16 106.3(4) . . ?
N3 C15 C17 109.2(5) . . ?
C16 C15 C17 109.8(6) . . ?
N3 C15 C18 108.6(5) . . ?
C16 C15 C18 112.2(6) . . ?
C17 C15 C18 110.7(6) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 C21 108.3(5) . . ?
N4 C19 C20 106.0(4) . . ?
C21 C19 C20 110.8(5) . . ?
N4 C19 C22 109.5(3) . . ?
C21 C19 C22 111.7(5) . . ?
C20 C19 C22 110.3(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22C 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22C C22 H22B 109.5 . . ?
C19 C22 H22A 109.5 . . ?
H22C C22 H22A 109.5 . . ?
H22B C22 H22A 109.5 . . ?
C26 C23 N5 111.2(6) . . ?
C26 C23 C25 115.3(8) . . ?
N5 C23 C25 108.8(6) . . ?
C26 C23 C24 114.8(10) . . ?
N5 C23 C24 104.6(6) . . ?
C25 C23 C24 101.3(9) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C27 C29 111.0(5) . . ?
N6 C27 C28 107.9(4) . . ?
C29 C27 C28 107.6(7) . . ?
N6 C27 C30 108.5(5) . . ?
C29 C27 C30 113.8(7) . . ?
C28 C27 C30 107.9(6) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
F3 C40 F1 108.5(4) . . ?
F3 C40 F2 107.3(3) . . ?
F1 C40 F2 107.9(4) . . ?
F3 C40 S1 110.8(3) . . ?
F1 C40 S1 111.0(3) . . ?
F2 C40 S1 111.1(3) . . ?
F5 C50 F4 109.6(5) . . ?
F5 C50 F6 106.1(5) . . ?
F4 C50 F6 108.0(5) . . ?
F5 C50 S2 112.1(4) . . ?
F4 C50 S2 111.3(3) . . ?
F6 C50 S2 109.6(4) . . ?
F9 C60 F7 109.4(4) . . ?
F9 C60 F8 107.7(3) . . ?
F7 C60 F8 106.4(4) . . ?
F9 C60 S3 111.8(3) . . ?
F7 C60 S3 111.3(3) . . ?
F8 C60 S3 110.0(3) . . ?
C1 N1 C7 164.1(4) . . ?
C2 N2 C11 166.6(3) . . ?
C3 N3 C15 164.6(5) . . ?
C4 N4 C19 170.5(4) . . ?
C5 N5 C23 163.7(5) . . ?
C6 N6 C27 168.1(5) . . ?
S1 O1 Li1 158.7(2) . . ?
S1 O2 Li2 138.2(2) . 1_655 ?
S2 O4 Li2 144.9(3) . . ?
S2 O6 Li1 147.9(2) . . ?
S3 O7 Li1 148.8(3) . . ?
S3 O9 Li2 140.1(2) . . ?
O1 S1 O2 113.82(15) . . ?
O1 S1 O3 114.21(14) . . ?
O2 S1 O3 115.46(13) . . ?
O1 S1 C40 103.18(19) . . ?
O2 S1 C40 104.37(17) . . ?
O3 S1 C40 103.85(18) . . ?
O6 S2 O4 116.05(18) . . ?
O6 S2 O5 113.9(2) . . ?
O4 S2 O5 113.64(19) . . ?
O6 S2 C50 103.7(2) . . ?
O4 S2 C50 104.6(2) . . ?
O5 S2 C50 103.0(2) . . ?
O8 S3 O9 115.08(18) . . ?
O8 S3 O7 115.93(19) . . ?
O9 S3 O7 114.01(16) . . ?
O8 S3 C60 103.92(18) . . ?
O9 S3 C60 102.93(18) . . ?
O7 S3 C60 102.48(19) . . ?
O7 Li1 O11 109.0(3) . . ?
O7 Li1 O1 117.7(3) . . ?
O11 Li1 O1 104.2(3) . . ?
O7 Li1 O6 112.5(3) . . ?
O11 Li1 O6 106.1(3) . . ?
O1 Li1 O6 106.6(3) . . ?
O9 Li2 O10 115.4(3) . . ?
O9 Li2 O4 109.2(3) . . ?
O10 Li2 O4 108.7(3) . . ?
O9 Li2 O2 108.7(3) . 1_455 ?
O10 Li2 O2 106.3(2) . 1_455 ?
O4 Li2 O2 108.4(3) . 1_455 ?

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
C10 C7 N1 C1 46.8(17) . . . . ?
C9 C7 N1 C1 166.2(14) . . . . ?
C8 C7 N1 C1 -77.0(16) . . . . ?
C12 C11 N2 C2 -107.5(15) . . . . ?
C13 C11 N2 C2 14.0(16) . . . . ?
C14 C11 N2 C2 131.9(14) . . . . ?
C16 C15 N3 C3 -60(2) . . . . ?
C17 C15 N3 C3 59(2) . . . . ?
C26 C23 N5 C5 101.2(18) . . . . ?
C25 C23 N5 C5 -27(2) . . . . ?
C24 C23 N5 C5 -134.3(17) . . . . ?
C29 C27 N6 C6 -113(2) . . . . ?
C28 C27 N6 C6 4(2) . . . . ?
C30 C27 N6 C6 121(2) . . . . ?
Li1 O1 S1 O2 -166.6(7) . . . . ?
Li1 O1 S1 O3 -31.0(7) . . . . ?
Li1 O1 S1 C40 81.0(7) . . . . ?
Li2 O2 S1 O1 136.4(3) 1_655 . . . ?
Li2 O2 S1 O3 1.5(4) 1_655 . . . ?
Li2 O2 S1 C40 -111.8(4) 1_655 . . . ?
F3 C40 S1 O1 175.9(3) . . . . ?
F1 C40 S1 O1 -63.4(3) . . . . ?
F2 C40 S1 O1 56.7(3) . . . . ?
F3 C40 S1 O2 56.6(3) . . . . ?
F1 C40 S1 O2 177.3(3) . . . . ?
F2 C40 S1 O2 -62.5(3) . . . . ?
F3 C40 S1 O3 -64.7(3) . . . . ?
F1 C40 S1 O3 56.0(3) . . . . ?
F2 C40 S1 O3 176.1(3) . . . . ?
Li1 O6 S2 O4 12.9(6) . . . . ?
Li1 O6 S2 O5 -121.9(5) . . . . ?
Li1 O6 S2 C50 126.9(5) . . . . ?
Li2 O4 S2 O6 -32.7(5) . . . . ?
Li2 O4 S2 O5 102.2(4) . . . . ?
Li2 O4 S2 C50 -146.3(4) . . . . ?
F5 C50 S2 O6 -58.2(5) . . . . ?
F4 C50 S2 O6 178.7(4) . . . . ?
F6 C50 S2 O6 59.3(4) . . . . ?
F5 C50 S2 O4 63.8(5) . . . . ?
F4 C50 S2 O4 -59.3(5) . . . . ?
F6 C50 S2 O4 -178.7(3) . . . . ?
F5 C50 S2 O5 -177.2(4) . . . . ?
F4 C50 S2 O5 59.7(5) . . . . ?
F6 C50 S2 O5 -59.7(4) . . . . ?
Li2 O9 S3 O8 120.2(4) . . . . ?
Li2 O9 S3 O7 -17.3(5) . . . . ?
Li2 O9 S3 C60 -127.4(4) . . . . ?
Li1 O7 S3 O8 -76.7(5) . . . . ?
Li1 O7 S3 O9 60.4(5) . . . . ?
Li1 O7 S3 C60 170.9(5) . . . . ?
F9 C60 S3 O8 -58.8(3) . . . . ?
F7 C60 S3 O8 178.5(3) . . . . ?
F8 C60 S3 O8 60.8(3) . . . . ?
F9 C60 S3 O9 -179.1(3) . . . . ?
F7 C60 S3 O9 58.2(3) . . . . ?
F8 C60 S3 O9 -59.6(3) . . . . ?
F9 C60 S3 O7 62.3(3) . . . . ?
F7 C60 S3 O7 -60.4(3) . . . . ?
F8 C60 S3 O7 -178.2(3) . . . . ?
S3 O7 Li1 O11 -132.8(4) . . . . ?
S3 O7 Li1 O1 109.0(5) . . . . ?
S3 O7 Li1 O6 -15.5(7) . . . . ?

_refine_diff_density_max         1.332
_refine_diff_density_min         -1.682
_refine_diff_density_rms         0.087

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_GIM280517
_database_code_depnum_ccdc_archive 'CCDC 1554402'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H49 Cl2 F6 P4 Re'
_chemical_formula_weight         1168.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   11.00550(4)
_cell_length_b                   18.56730(7)
_cell_length_c                   24.45640(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4997.48(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    47720
_cell_measurement_theta_min      2.985
_cell_measurement_theta_max      79.389

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_F_000             2336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    7.435
_shelx_estimated_absorpt_T_min   0.332
_shelx_estimated_absorpt_T_max   0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.73035
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            57867
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.988
_diffrn_reflns_theta_max         79.687
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10772
_reflns_number_gt                10651
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_max     0.984
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.27e (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27e (Rigaku OD, 2015)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0420P)²+8.3449P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_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 x determined using 4649 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10772
_refine_ls_number_parameters     587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0830
_refine_ls_wR_factor_gt          0.0828
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.17413(2) 0.14554(2) 0.63295(2) 0.02695(7) Uani 1 1 d . . . . .
C1 C 0.2666(6) 0.1397(4) 0.5514(2) 0.0376(12) Uani 1 1 d . . . . .
H1A H 0.3021 0.0991 0.5339 0.045 Uiso 1 1 calc R U . . .
C2 C 0.1441(6) 0.1558(3) 0.5429(2) 0.0329(12) Uani 1 1 d . . . . .
H2A H 0.0933 0.1224 0.5243 0.039 Uiso 1 1 calc R U . . .
C3 C 0.0945(5) 0.2226(3) 0.5620(2) 0.0320(11) Uani 1 1 d . . . . .
C4 C -0.0263(6) 0.2456(4) 0.5478(3) 0.0383(13) Uani 1 1 d . . . . .
H4A H -0.0781 0.2144 0.5277 0.046 Uiso 1 1 calc R U . . .
C5 C -0.0670(6) 0.3121(4) 0.5632(3) 0.0426(14) Uani 1 1 d . . . . .
H5A H -0.1471 0.3267 0.5539 0.051 Uiso 1 1 calc R U . . .
C6 C 0.0086(7) 0.3595(4) 0.5928(3) 0.0462(15) Uani 1 1 d . . . . .
H6A H -0.0200 0.4063 0.6017 0.055 Uiso 1 1 calc R U . . .
C7 C 0.1214(7) 0.3392(3) 0.6087(3) 0.0422(14) Uani 1 1 d . . . . .
H7A H 0.1702 0.3713 0.6295 0.051 Uiso 1 1 calc R U . . .
C8 C 0.1680(6) 0.2687(3) 0.5943(2) 0.0351(11) Uani 1 1 d . . . . .
C9 C 0.2875(6) 0.2444(3) 0.6100(3) 0.0368(13) Uani 1 1 d . . . . .
H9A H 0.3321 0.2700 0.6370 0.044 Uiso 1 1 calc R U . . .
C10 C 0.3374(6) 0.1835(3) 0.5858(2) 0.0379(13) Uani 1 1 d . . . . .
H10A H 0.4199 0.1714 0.5926 0.045 Uiso 1 1 calc R U . . .
C11 C 0.2308(6) 0.2402(4) 0.7636(2) 0.0374(13) Uani 1 1 d . . . . .
C12 C 0.3008(8) 0.2233(5) 0.8089(3) 0.057(2) Uani 1 1 d . . . . .
H12A H 0.3021 0.1752 0.8220 0.068 Uiso 1 1 calc R U . . .
C13 C 0.3689(10) 0.2754(5) 0.8353(4) 0.073(3) Uani 1 1 d . . . . .
H13A H 0.4145 0.2632 0.8670 0.087 Uiso 1 1 calc R U . . .
C14 C 0.3702(8) 0.3446(5) 0.8157(4) 0.066(2) Uani 1 1 d . . . . .
H14A H 0.4199 0.3799 0.8327 0.079 Uiso 1 1 calc R U . . .
C15 C 0.2988(8) 0.3629(5) 0.7709(4) 0.061(2) Uani 1 1 d . . . . .
H15A H 0.2968 0.4112 0.7581 0.073 Uiso 1 1 calc R U . . .
C16 C 0.2310(7) 0.3103(4) 0.7454(3) 0.0503(17) Uani 1 1 d . . . . .
H16A H 0.1833 0.3227 0.7144 0.060 Uiso 1 1 calc R U . . .
C17 C -0.0118(5) 0.2228(3) 0.7409(2) 0.0327(11) Uani 1 1 d . . . . .
C18 C -0.0771(6) 0.2542(3) 0.6986(3) 0.0354(12) Uani 1 1 d . . . . .
H18A H -0.0505 0.2481 0.6619 0.042 Uiso 1 1 calc R U . . .
C19 C -0.1816(6) 0.2946(3) 0.7094(3) 0.0422(13) Uani 1 1 d . . . . .
H19A H -0.2255 0.3162 0.6802 0.051 Uiso 1 1 calc R U . . .
C20 C -0.2206(6) 0.3030(3) 0.7626(3) 0.0438(15) Uani 1 1 d . . . . .
H20A H -0.2916 0.3304 0.7700 0.053 Uiso 1 1 calc R U . . .
C21 C -0.1563(7) 0.2717(4) 0.8055(3) 0.0467(16) Uani 1 1 d . . . . .
H21A H -0.1836 0.2772 0.8421 0.056 Uiso 1 1 calc R U . . .
C22 C -0.0529(7) 0.2328(4) 0.7945(3) 0.0425(14) Uani 1 1 d . . . . .
H22A H -0.0084 0.2123 0.8239 0.051 Uiso 1 1 calc R U . . .
C23 C 0.3663(5) -0.0124(3) 0.6266(3) 0.0331(11) Uani 1 1 d . . . . .
C24 C 0.3271(7) -0.0816(3) 0.6155(3) 0.0399(12) Uani 1 1 d . . . . .
H24A H 0.2562 -0.0993 0.6331 0.048 Uiso 1 1 calc R U . . .
C25 C 0.3896(7) -0.1258(4) 0.5792(3) 0.0496(17) Uani 1 1 d . . . . .
H25A H 0.3614 -0.1733 0.5723 0.059 Uiso 1 1 calc R U . . .
C26 C 0.4926(8) -0.1007(4) 0.5530(3) 0.0533(18) Uani 1 1 d . . . . .
H26A H 0.5346 -0.1300 0.5274 0.064 Uiso 1 1 calc R U . . .
C27 C 0.5332(8) -0.0317(4) 0.5650(4) 0.0541(19) Uani 1 1 d . . . . .
H27A H 0.6046 -0.0141 0.5478 0.065 Uiso 1 1 calc R U . . .
C60 C -0.1840(14) -0.0838(6) 0.4304(6) 0.098(4) Uani 1 1 d . . . . .
H60A H -0.1161 -0.0725 0.4053 0.118 Uiso 1 1 calc R U . . .
H60B H -0.1630 -0.0649 0.4671 0.118 Uiso 1 1 calc R U . . .
C28 C 0.4720(7) 0.0116(4) 0.6013(3) 0.0458(15) Uani 1 1 d . . . . .
H28A H 0.5022 0.0583 0.6093 0.055 Uiso 1 1 calc R U . . .
C29 C 0.4172(6) 0.0782(4) 0.7141(2) 0.0349(12) Uani 1 1 d . . . . .
C30 C 0.4826(7) 0.0277(4) 0.7442(3) 0.0442(15) Uani 1 1 d . . . . .
H30A H 0.4571 -0.0211 0.7449 0.053 Uiso 1 1 calc R U . . .
C31 C 0.5857(7) 0.0489(4) 0.7734(3) 0.0485(16) Uani 1 1 d . . . . .
H31A H 0.6291 0.0144 0.7944 0.058 Uiso 1 1 calc R U . . .
C32 C 0.6251(7) 0.1192(4) 0.7720(3) 0.0491(17) Uani 1 1 d . . . . .
H32A H 0.6966 0.1329 0.7912 0.059 Uiso 1 1 calc R U . . .
C33 C 0.5597(7) 0.1700(4) 0.7424(3) 0.0492(17) Uani 1 1 d . . . . .
H33A H 0.5855 0.2188 0.7416 0.059 Uiso 1 1 calc R U . . .
C34 C 0.4570(5) 0.1492(4) 0.7140(3) 0.0388(13) Uani 1 1 d . . . . .
H34A H 0.4126 0.1842 0.6939 0.047 Uiso 1 1 calc R U . . .
C35 C -0.1342(5) 0.0924(3) 0.6063(3) 0.0346(12) Uani 1 1 d . . . . .
C36 C -0.2166(5) 0.1350(3) 0.6347(3) 0.0410(13) Uani 1 1 d . . . . .
H36A H -0.2078 0.1418 0.6730 0.049 Uiso 1 1 calc R U . . .
C37 C -0.3124(6) 0.1676(4) 0.6068(3) 0.0454(15) Uani 1 1 d . . . . .
H37A H -0.3665 0.1984 0.6259 0.055 Uiso 1 1 calc R U . . .
C38 C -0.3293(6) 0.1553(4) 0.5512(3) 0.0505(16) Uani 1 1 d . . . . .
H38A H -0.3947 0.1776 0.5323 0.061 Uiso 1 1 calc R U . . .
C39 C -0.2498(6) 0.1103(4) 0.5237(3) 0.0460(16) Uani 1 1 d . . . . .
H39A H -0.2623 0.1002 0.4860 0.055 Uiso 1 1 calc R U . . .
C40 C -0.1522(6) 0.0798(4) 0.5510(3) 0.0416(14) Uani 1 1 d . . . . .
H40A H -0.0969 0.0499 0.5316 0.050 Uiso 1 1 calc R U . . .
C41 C 0.0235(6) -0.0242(3) 0.6021(3) 0.0393(13) Uani 1 1 d . . . . .
C42 C -0.0497(9) -0.0821(4) 0.6165(3) 0.056(2) Uani 1 1 d . . . . .
H42A H -0.1016 -0.0787 0.6474 0.068 Uiso 1 1 calc R U . . .
C43 C -0.0471(10) -0.1450(5) 0.5859(4) 0.069(2) Uani 1 1 d . . . . .
H43A H -0.0959 -0.1847 0.5967 0.083 Uiso 1 1 calc R U . . .
C44 C 0.0256(10) -0.1506(5) 0.5400(4) 0.066(2) Uani 1 1 d . . . . .
H44A H 0.0263 -0.1937 0.5191 0.079 Uiso 1 1 calc R U . . .
C45 C 0.0960(8) -0.0936(5) 0.5250(4) 0.058(2) Uani 1 1 d . . . . .
H45A H 0.1456 -0.0967 0.4932 0.069 Uiso 1 1 calc R U . . .
C46 C 0.0953(7) -0.0307(4) 0.5562(3) 0.0433(15) Uani 1 1 d . . . . .
H46A H 0.1454 0.0085 0.5456 0.052 Uiso 1 1 calc R U . . .
C50 C 0.1262(6) 0.0977(3) 0.7727(2) 0.0369(12) Uani 1 1 d . . . . .
H50A H 0.2077 0.0908 0.7890 0.044 Uiso 1 1 calc R U . . .
H50B H 0.0692 0.1091 0.8028 0.044 Uiso 1 1 calc R U . . .
C51 C 0.1950(5) -0.0085(3) 0.7165(2) 0.0337(12) Uani 1 1 d . . . . .
H51B H 0.1642 -0.0489 0.6940 0.040 Uiso 1 1 calc R U . . .
H51A H 0.2500 -0.0292 0.7445 0.040 Uiso 1 1 calc R U . . .
C52 C -0.0265(6) 0.0376(3) 0.7086(2) 0.0359(12) Uani 1 1 d . . . . .
H52A H -0.0787 0.0754 0.7249 0.043 Uiso 1 1 calc R U . . .
H52B H -0.0740 -0.0076 0.7077 0.043 Uiso 1 1 calc R U . . .
C53 C 0.0863(6) 0.0264(3) 0.7461(2) 0.0331(12) Uani 1 1 d . . . . .
C54 C 0.0472(7) -0.0245(4) 0.7922(3) 0.0418(14) Uani 1 1 d . . . . .
H54C H 0.0247 -0.0713 0.7767 0.063 Uiso 1 1 calc R U . . .
H54B H -0.0227 -0.0039 0.8114 0.063 Uiso 1 1 calc R U . . .
H54A H 0.1147 -0.0308 0.8179 0.063 Uiso 1 1 calc R U . . .
F1 F 0.0610(10) -0.0018(5) 0.3777(5) 0.161(5) Uani 1 1 d . . . . .
F2 F 0.1847(10) 0.0819(10) 0.4188(6) 0.247(9) Uani 1 1 d . . . . .
F3 F 0.0030(12) 0.0708(9) 0.4417(3) 0.220(8) Uani 1 1 d . . . . .
F4 F 0.0667(15) 0.1628(5) 0.4000(6) 0.205(7) Uani 1 1 d . . . . .
F5 F -0.0642(8) 0.0843(5) 0.3588(4) 0.129(3) Uani 1 1 d . . . . .
F6 F 0.1349(13) 0.0791(8) 0.3357(4) 0.200(7) Uani 1 1 d . . . . .
P1 P 0.13249(13) 0.17588(8) 0.72579(6) 0.0301(3) Uani 1 1 d . . . . .
P2 P 0.28513(13) 0.05203(7) 0.67184(6) 0.0292(3) Uani 1 1 d . . . . .
P3 P 0.01074(12) 0.06371(7) 0.63782(6) 0.0298(3) Uani 1 1 d . . . . .
P4 P 0.0618(2) 0.08459(16) 0.38809(9) 0.0712(7) Uani 1 1 d . . . . .
Cl1 Cl -0.2027(8) -0.1748(2) 0.4340(3) 0.227(4) Uani 1 1 d . . . . .
Cl2 Cl -0.3150(4) -0.0427(2) 0.40735(19) 0.1200(12) 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
Re1 C2 2.236(5) . ?
Re1 C1 2.242(5) . ?
Re1 C10 2.248(6) . ?
Re1 C9 2.289(6) . ?
Re1 P2 2.3264(14) . ?
Re1 P3 2.3572(13) . ?
Re1 P1 2.3840(15) . ?
Re1 C3 2.413(6) . ?
Re1 C8 2.476(5) . ?
C1 C2 1.397(9) . ?
C1 C10 1.408(9) . ?
C1 H1A 0.9500 . ?
C2 C3 1.433(9) . ?
C2 H2A 0.9500 . ?
C3 C8 1.418(8) . ?
C3 C4 1.439(9) . ?
C4 C5 1.366(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.409(11) . ?
C5 H5A 0.9500 . ?
C6 C7 1.355(10) . ?
C6 H6A 0.9500 . ?
C7 C8 1.448(9) . ?
C7 H7A 0.9500 . ?
C8 C9 1.443(9) . ?
C9 C10 1.389(9) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C16 1.376(10) . ?
C11 C12 1.384(10) . ?
C11 P1 1.858(6) . ?
C12 C13 1.384(11) . ?
C12 H12A 0.9500 . ?
C13 C14 1.372(14) . ?
C13 H13A 0.9500 . ?
C14 C15 1.390(13) . ?
C14 H14A 0.9500 . ?
C15 C16 1.380(10) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 C18 1.388(9) . ?
C17 C22 1.399(9) . ?
C17 P1 1.848(6) . ?
C18 C19 1.399(9) . ?
C18 H18A 0.9500 . ?
C19 C20 1.380(10) . ?
C19 H19A 0.9500 . ?
C20 C21 1.393(11) . ?
C20 H20A 0.9500 . ?
C21 C22 1.374(10) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C24 1.382(8) . ?
C23 C28 1.390(9) . ?
C23 P2 1.858(6) . ?
C24 C25 1.391(10) . ?
C24 H24A 0.9500 . ?
C25 C26 1.382(12) . ?
C25 H25A 0.9500 . ?
C26 C27 1.388(12) . ?
C26 H26A 0.9500 . ?
C27 C28 1.375(11) . ?
C27 H27A 0.9500 . ?
C60 Cl1 1.705(12) . ?
C60 Cl2 1.726(14) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C28 H28A 0.9500 . ?
C29 C34 1.388(9) . ?
C29 C30 1.392(9) . ?
C29 P2 1.849(6) . ?
C30 C31 1.396(10) . ?
C30 H30A 0.9500 . ?
C31 C32 1.375(11) . ?
C31 H31A 0.9500 . ?
C32 C33 1.391(11) . ?
C32 H32A 0.9500 . ?
C33 C34 1.382(9) . ?
C33 H33A 0.9500 . ?
C34 H34A 0.9500 . ?
C35 C40 1.387(9) . ?
C35 C36 1.388(9) . ?
C35 P3 1.850(6) . ?
C36 C37 1.394(9) . ?
C36 H36A 0.9500 . ?
C37 C38 1.391(11) . ?
C37 H37A 0.9500 . ?
C38 C39 1.384(11) . ?
C38 H38A 0.9500 . ?
C39 C40 1.386(9) . ?
C39 H39A 0.9500 . ?
C40 H40A 0.9500 . ?
C41 C46 1.378(10) . ?
C41 C42 1.389(10) . ?
C41 P3 1.858(7) . ?
C42 C43 1.386(12) . ?
C42 H42A 0.9500 . ?
C43 C44 1.384(14) . ?
C43 H43A 0.9500 . ?
C44 C45 1.362(13) . ?
C44 H44A 0.9500 . ?
C45 C46 1.395(10) . ?
C45 H45A 0.9500 . ?
C46 H46A 0.9500 . ?
C50 C53 1.539(9) . ?
C50 P1 1.852(6) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C53 1.540(9) . ?
C51 P2 1.855(6) . ?
C51 H51B 0.9900 . ?
C51 H51A 0.9900 . ?
C52 C53 1.558(8) . ?
C52 P3 1.843(6) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.532(8) . ?
C54 H54C 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54A 0.9800 . ?
F1 P4 1.624(9) . ?
F2 P4 1.548(11) . ?
F3 P4 1.484(8) . ?
F4 P4 1.482(8) . ?
F5 P4 1.560(8) . ?
F6 P4 1.517(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
C2 Re1 C1 36.4(2) . . ?
C2 Re1 C10 65.6(2) . . ?
C1 Re1 C10 36.5(2) . . ?
C2 Re1 C9 76.8(2) . . ?
C1 Re1 C9 64.8(2) . . ?
C10 Re1 C9 35.6(2) . . ?
C2 Re1 P2 122.99(16) . . ?
C1 Re1 P2 95.13(18) . . ?
C10 Re1 P2 91.38(17) . . ?
C9 Re1 P2 114.35(17) . . ?
C2 Re1 P3 89.55(16) . . ?
C1 Re1 P3 111.09(18) . . ?
C10 Re1 P3 146.93(17) . . ?
C9 Re1 P3 160.92(16) . . ?
P2 Re1 P3 84.20(5) . . ?
C2 Re1 P1 152.84(16) . . ?
C1 Re1 P1 161.12(18) . . ?
C10 Re1 P1 124.58(17) . . ?
C9 Re1 P1 98.53(17) . . ?
P2 Re1 P1 83.56(5) . . ?
P3 Re1 P1 87.56(5) . . ?
C2 Re1 C3 35.6(2) . . ?
C1 Re1 C3 63.5(2) . . ?
C10 Re1 C3 74.7(2) . . ?
C9 Re1 C3 63.0(2) . . ?
P2 Re1 C3 157.98(15) . . ?
P3 Re1 C3 98.14(14) . . ?
P1 Re1 C3 118.34(15) . . ?
C2 Re1 C8 62.7(2) . . ?
C1 Re1 C8 73.6(2) . . ?
C10 Re1 C8 62.4(2) . . ?
C9 Re1 C8 35.0(2) . . ?
P2 Re1 C8 149.31(17) . . ?
P3 Re1 C8 126.44(16) . . ?
P1 Re1 C8 98.05(14) . . ?
C3 Re1 C8 33.7(2) . . ?
C2 C1 C10 119.9(6) . . ?
C2 C1 Re1 71.6(3) . . ?
C10 C1 Re1 71.9(3) . . ?
C2 C1 H1A 120.0 . . ?
C10 C1 H1A 120.0 . . ?
Re1 C1 H1A 128.7 . . ?
C1 C2 C3 120.3(6) . . ?
C1 C2 Re1 72.1(3) . . ?
C3 C2 Re1 79.0(3) . . ?
C1 C2 H2A 119.8 . . ?
C3 C2 H2A 119.8 . . ?
Re1 C2 H2A 120.1 . . ?
C8 C3 C2 119.2(6) . . ?
C8 C3 C4 118.8(6) . . ?
C2 C3 C4 122.0(6) . . ?
C8 C3 Re1 75.6(3) . . ?
C2 C3 Re1 65.4(3) . . ?
C4 C3 Re1 133.2(4) . . ?
C5 C4 C3 120.3(6) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C4 C5 C6 120.8(6) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
C7 C6 C5 121.0(6) . . ?
C7 C6 H6A 119.5 . . ?
C5 C6 H6A 119.5 . . ?
C6 C7 C8 120.4(7) . . ?
C6 C7 H7A 119.8 . . ?
C8 C7 H7A 119.8 . . ?
C3 C8 C9 118.6(5) . . ?
C3 C8 C7 118.6(6) . . ?
C9 C8 C7 122.7(6) . . ?
C3 C8 Re1 70.7(3) . . ?
C9 C8 Re1 65.4(3) . . ?
C7 C8 Re1 138.7(4) . . ?
C10 C9 C8 120.1(6) . . ?
C10 C9 Re1 70.6(3) . . ?
C8 C9 Re1 79.6(3) . . ?
C10 C9 H9A 120.0 . . ?
C8 C9 H9A 120.0 . . ?
Re1 C9 H9A 120.9 . . ?
C9 C10 C1 120.5(6) . . ?
C9 C10 Re1 73.8(3) . . ?
C1 C10 Re1 71.5(3) . . ?
C9 C10 H10A 119.8 . . ?
C1 C10 H10A 119.8 . . ?
Re1 C10 H10A 126.9 . . ?
C16 C11 C12 118.2(6) . . ?
C16 C11 P1 116.6(5) . . ?
C12 C11 P1 125.2(6) . . ?
C13 C12 C11 121.2(8) . . ?
C13 C12 H12A 119.4 . . ?
C11 C12 H12A 119.4 . . ?
C14 C13 C12 119.7(8) . . ?
C14 C13 H13A 120.1 . . ?
C12 C13 H13A 120.1 . . ?
C13 C14 C15 120.0(7) . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C16 C15 C14 119.2(8) . . ?
C16 C15 H15A 120.4 . . ?
C14 C15 H15A 120.4 . . ?
C11 C16 C15 121.6(7) . . ?
C11 C16 H16A 119.2 . . ?
C15 C16 H16A 119.2 . . ?
C18 C17 C22 118.4(6) . . ?
C18 C17 P1 119.6(5) . . ?
C22 C17 P1 121.8(5) . . ?
C17 C18 C19 120.7(6) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C20 C19 C18 119.6(6) . . ?
C20 C19 H19A 120.2 . . ?
C18 C19 H19A 120.2 . . ?
C19 C20 C21 120.4(6) . . ?
C19 C20 H20A 119.8 . . ?
C21 C20 H20A 119.8 . . ?
C22 C21 C20 119.5(6) . . ?
C22 C21 H21A 120.2 . . ?
C20 C21 H21A 120.2 . . ?
C21 C22 C17 121.4(6) . . ?
C21 C22 H22A 119.3 . . ?
C17 C22 H22A 119.3 . . ?
C24 C23 C28 118.1(6) . . ?
C24 C23 P2 124.4(5) . . ?
C28 C23 P2 117.5(5) . . ?
C23 C24 C25 121.3(7) . . ?
C23 C24 H24A 119.4 . . ?
C25 C24 H24A 119.4 . . ?
C26 C25 C24 120.2(7) . . ?
C26 C25 H25A 119.9 . . ?
C24 C25 H25A 119.9 . . ?
C25 C26 C27 118.5(7) . . ?
C25 C26 H26A 120.8 . . ?
C27 C26 H26A 120.8 . . ?
C28 C27 C26 121.2(7) . . ?
C28 C27 H27A 119.4 . . ?
C26 C27 H27A 119.4 . . ?
Cl1 C60 Cl2 110.8(8) . . ?
Cl1 C60 H60A 109.5 . . ?
Cl2 C60 H60A 109.5 . . ?
Cl1 C60 H60B 109.5 . . ?
Cl2 C60 H60B 109.5 . . ?
H60A C60 H60B 108.1 . . ?
C27 C28 C23 120.7(7) . . ?
C27 C28 H28A 119.7 . . ?
C23 C28 H28A 119.7 . . ?
C34 C29 C30 118.5(6) . . ?
C34 C29 P2 119.7(5) . . ?
C30 C29 P2 121.7(5) . . ?
C29 C30 C31 120.0(7) . . ?
C29 C30 H30A 120.0 . . ?
C31 C30 H30A 120.0 . . ?
C32 C31 C30 120.7(7) . . ?
C32 C31 H31A 119.6 . . ?
C30 C31 H31A 119.6 . . ?
C31 C32 C33 119.5(7) . . ?
C31 C32 H32A 120.2 . . ?
C33 C32 H32A 120.2 . . ?
C34 C33 C32 119.7(7) . . ?
C34 C33 H33A 120.2 . . ?
C32 C33 H33A 120.2 . . ?
C33 C34 C29 121.5(7) . . ?
C33 C34 H34A 119.2 . . ?
C29 C34 H34A 119.2 . . ?
C40 C35 C36 119.3(6) . . ?
C40 C35 P3 118.7(5) . . ?
C36 C35 P3 121.3(5) . . ?
C35 C36 C37 119.8(7) . . ?
C35 C36 H36A 120.1 . . ?
C37 C36 H36A 120.1 . . ?
C38 C37 C36 120.6(7) . . ?
C38 C37 H37A 119.7 . . ?
C36 C37 H37A 119.7 . . ?
C39 C38 C37 119.3(6) . . ?
C39 C38 H38A 120.4 . . ?
C37 C38 H38A 120.4 . . ?
C38 C39 C40 120.2(7) . . ?
C38 C39 H39A 119.9 . . ?
C40 C39 H39A 119.9 . . ?
C39 C40 C35 120.7(7) . . ?
C39 C40 H40A 119.6 . . ?
C35 C40 H40A 119.6 . . ?
C46 C41 C42 118.2(7) . . ?
C46 C41 P3 120.2(5) . . ?
C42 C41 P3 121.1(6) . . ?
C43 C42 C41 120.1(8) . . ?
C43 C42 H42A 119.9 . . ?
C41 C42 H42A 119.9 . . ?
C44 C43 C42 120.9(8) . . ?
C44 C43 H43A 119.5 . . ?
C42 C43 H43A 119.5 . . ?
C45 C44 C43 119.3(8) . . ?
C45 C44 H44A 120.4 . . ?
C43 C44 H44A 120.4 . . ?
C44 C45 C46 120.0(9) . . ?
C44 C45 H45A 120.0 . . ?
C46 C45 H45A 120.0 . . ?
C41 C46 C45 121.5(7) . . ?
C41 C46 H46A 119.3 . . ?
C45 C46 H46A 119.3 . . ?
C53 C50 P1 115.0(4) . . ?
C53 C50 H50A 108.5 . . ?
P1 C50 H50A 108.5 . . ?
C53 C50 H50B 108.5 . . ?
P1 C50 H50B 108.5 . . ?
H50A C50 H50B 107.5 . . ?
C53 C51 P2 115.9(4) . . ?
C53 C51 H51B 108.3 . . ?
P2 C51 H51B 108.3 . . ?
C53 C51 H51A 108.3 . . ?
P2 C51 H51A 108.3 . . ?
H51B C51 H51A 107.4 . . ?
C53 C52 P3 114.3(4) . . ?
C53 C52 H52A 108.7 . . ?
P3 C52 H52A 108.7 . . ?
C53 C52 H52B 108.7 . . ?
P3 C52 H52B 108.7 . . ?
H52A C52 H52B 107.6 . . ?
C54 C53 C50 107.4(5) . . ?
C54 C53 C51 107.7(5) . . ?
C50 C53 C51 109.8(5) . . ?
C54 C53 C52 107.0(5) . . ?
C50 C53 C52 111.2(5) . . ?
C51 C53 C52 113.5(5) . . ?
C53 C54 H54C 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54C C54 H54B 109.5 . . ?
C53 C54 H54A 109.5 . . ?
H54C C54 H54A 109.5 . . ?
H54B C54 H54A 109.5 . . ?
C17 P1 C50 102.3(3) . . ?
C17 P1 C11 95.6(3) . . ?
C50 P1 C11 102.6(3) . . ?
C17 P1 Re1 117.8(2) . . ?
C50 P1 Re1 114.3(2) . . ?
C11 P1 Re1 120.9(2) . . ?
C29 P2 C51 104.5(3) . . ?
C29 P2 C23 97.2(3) . . ?
C51 P2 C23 102.6(3) . . ?
C29 P2 Re1 116.4(2) . . ?
C51 P2 Re1 114.35(19) . . ?
C23 P2 Re1 119.3(2) . . ?
C52 P3 C35 106.0(3) . . ?
C52 P3 C41 103.2(3) . . ?
C35 P3 C41 97.0(3) . . ?
C52 P3 Re1 112.7(2) . . ?
C35 P3 Re1 116.81(19) . . ?
C41 P3 Re1 119.0(2) . . ?
F4 P4 F3 90.7(9) . . ?
F4 P4 F6 102.2(9) . . ?
F3 P4 F6 165.1(10) . . ?
F4 P4 F2 84.5(8) . . ?
F3 P4 F2 86.9(8) . . ?
F6 P4 F2 86.8(8) . . ?
F4 P4 F5 97.3(7) . . ?
F3 P4 F5 91.0(7) . . ?
F6 P4 F5 94.8(7) . . ?
F2 P4 F5 177.3(9) . . ?
F4 P4 F1 177.1(7) . . ?
F3 P4 F1 88.1(8) . . ?
F6 P4 F1 78.7(7) . . ?
F2 P4 F1 92.8(8) . . ?
F5 P4 F1 85.4(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
C10 C1 C2 C3 9.7(8) . . . . ?
Re1 C1 C2 C3 65.0(5) . . . . ?
C10 C1 C2 Re1 -55.3(5) . . . . ?
C1 C2 C3 C8 -6.2(8) . . . . ?
Re1 C2 C3 C8 55.3(5) . . . . ?
C1 C2 C3 C4 171.5(5) . . . . ?
Re1 C2 C3 C4 -127.0(5) . . . . ?
C1 C2 C3 Re1 -61.5(4) . . . . ?
C8 C3 C4 C5 2.9(9) . . . . ?
C2 C3 C4 C5 -174.8(6) . . . . ?
Re1 C3 C4 C5 100.2(7) . . . . ?
C3 C4 C5 C6 0.4(9) . . . . ?
C4 C5 C6 C7 -2.8(10) . . . . ?
C5 C6 C7 C8 1.7(10) . . . . ?
C2 C3 C8 C9 -4.4(8) . . . . ?
C4 C3 C8 C9 177.8(5) . . . . ?
Re1 C3 C8 C9 46.1(5) . . . . ?
C2 C3 C8 C7 173.8(5) . . . . ?
C4 C3 C8 C7 -4.0(8) . . . . ?
Re1 C3 C8 C7 -135.7(5) . . . . ?
C2 C3 C8 Re1 -50.5(4) . . . . ?
C4 C3 C8 Re1 131.7(5) . . . . ?
C6 C7 C8 C3 1.8(9) . . . . ?
C6 C7 C8 C9 179.9(6) . . . . ?
C6 C7 C8 Re1 -91.2(8) . . . . ?
C3 C8 C9 C10 11.7(8) . . . . ?
C7 C8 C9 C10 -166.4(5) . . . . ?
Re1 C8 C9 C10 60.2(5) . . . . ?
C3 C8 C9 Re1 -48.5(5) . . . . ?
C7 C8 C9 Re1 133.4(5) . . . . ?
C8 C9 C10 C1 -8.4(8) . . . . ?
Re1 C9 C10 C1 56.4(5) . . . . ?
C8 C9 C10 Re1 -64.8(5) . . . . ?
C2 C1 C10 C9 -2.3(8) . . . . ?
Re1 C1 C10 C9 -57.5(5) . . . . ?
C2 C1 C10 Re1 55.1(5) . . . . ?
C16 C11 C12 C13 0.3(13) . . . . ?
P1 C11 C12 C13 -178.2(8) . . . . ?
C11 C12 C13 C14 -1.9(16) . . . . ?
C12 C13 C14 C15 3.0(16) . . . . ?
C13 C14 C15 C16 -2.6(15) . . . . ?
C12 C11 C16 C15 0.2(12) . . . . ?
P1 C11 C16 C15 178.8(7) . . . . ?
C14 C15 C16 C11 1.0(14) . . . . ?
C22 C17 C18 C19 -0.2(9) . . . . ?
P1 C17 C18 C19 -175.1(5) . . . . ?
C17 C18 C19 C20 -0.4(10) . . . . ?
C18 C19 C20 C21 0.2(10) . . . . ?
C19 C20 C21 C22 0.6(10) . . . . ?
C20 C21 C22 C17 -1.2(11) . . . . ?
C18 C17 C22 C21 1.0(10) . . . . ?
P1 C17 C22 C21 175.8(5) . . . . ?
C28 C23 C24 C25 -1.6(10) . . . . ?
P2 C23 C24 C25 177.0(6) . . . . ?
C23 C24 C25 C26 -0.3(11) . . . . ?
C24 C25 C26 C27 1.7(12) . . . . ?
C25 C26 C27 C28 -1.0(13) . . . . ?
C26 C27 C28 C23 -0.9(13) . . . . ?
C24 C23 C28 C27 2.2(11) . . . . ?
P2 C23 C28 C27 -176.4(6) . . . . ?
C34 C29 C30 C31 0.0(11) . . . . ?
P2 C29 C30 C31 176.6(6) . . . . ?
C29 C30 C31 C32 -1.2(12) . . . . ?
C30 C31 C32 C33 1.6(12) . . . . ?
C31 C32 C33 C34 -1.0(12) . . . . ?
C32 C33 C34 C29 -0.2(11) . . . . ?
C30 C29 C34 C33 0.6(10) . . . . ?
P2 C29 C34 C33 -176.0(6) . . . . ?
C40 C35 C36 C37 -3.5(9) . . . . ?
P3 C35 C36 C37 167.1(5) . . . . ?
C35 C36 C37 C38 2.9(10) . . . . ?
C36 C37 C38 C39 -0.1(10) . . . . ?
C37 C38 C39 C40 -2.2(10) . . . . ?
C38 C39 C40 C35 1.6(10) . . . . ?
C36 C35 C40 C39 1.2(9) . . . . ?
P3 C35 C40 C39 -169.6(5) . . . . ?
C46 C41 C42 C43 1.6(12) . . . . ?
P3 C41 C42 C43 173.7(7) . . . . ?
C41 C42 C43 C44 -1.6(15) . . . . ?
C42 C43 C44 C45 0.5(15) . . . . ?
C43 C44 C45 C46 0.7(14) . . . . ?
C42 C41 C46 C45 -0.5(11) . . . . ?
P3 C41 C46 C45 -172.7(6) . . . . ?
C44 C45 C46 C41 -0.7(13) . . . . ?
P1 C50 C53 C54 -162.2(5) . . . . ?
P1 C50 C53 C51 81.0(6) . . . . ?
P1 C50 C53 C52 -45.5(6) . . . . ?
P2 C51 C53 C54 -164.1(4) . . . . ?
P2 C51 C53 C50 -47.5(6) . . . . ?
P2 C51 C53 C52 77.7(6) . . . . ?
P3 C52 C53 C54 -155.8(4) . . . . ?
P3 C52 C53 C50 87.2(6) . . . . ?
P3 C52 C53 C51 -37.2(6) . . . . ?
C18 C17 P1 C50 -141.6(5) . . . . ?
C22 C17 P1 C50 43.6(6) . . . . ?
C18 C17 P1 C11 114.2(5) . . . . ?
C22 C17 P1 C11 -60.6(6) . . . . ?
C18 C17 P1 Re1 -15.3(6) . . . . ?
C22 C17 P1 Re1 169.9(5) . . . . ?
C53 C50 P1 C17 100.1(5) . . . . ?
C53 C50 P1 C11 -161.2(5) . . . . ?
C53 C50 P1 Re1 -28.5(5) . . . . ?
C16 C11 P1 C17 -61.6(6) . . . . ?
C12 C11 P1 C17 116.9(7) . . . . ?
C16 C11 P1 C50 -165.6(6) . . . . ?
C12 C11 P1 C50 12.9(7) . . . . ?
C16 C11 P1 Re1 65.7(6) . . . . ?
C12 C11 P1 Re1 -115.8(6) . . . . ?
C34 C29 P2 C51 -137.6(5) . . . . ?
C30 C29 P2 C51 45.9(6) . . . . ?
C34 C29 P2 C23 117.3(5) . . . . ?
C30 C29 P2 C23 -59.2(6) . . . . ?
C34 C29 P2 Re1 -10.5(6) . . . . ?
C30 C29 P2 Re1 173.0(5) . . . . ?
C53 C51 P2 C29 98.4(5) . . . . ?
C53 C51 P2 C23 -160.6(4) . . . . ?
C53 C51 P2 Re1 -30.0(5) . . . . ?
C24 C23 P2 C29 130.2(6) . . . . ?
C28 C23 P2 C29 -51.2(6) . . . . ?
C24 C23 P2 C51 23.6(6) . . . . ?
C28 C23 P2 C51 -157.9(6) . . . . ?
C24 C23 P2 Re1 -104.0(5) . . . . ?
C28 C23 P2 Re1 74.5(6) . . . . ?
C53 C52 P3 C35 -168.2(4) . . . . ?
C53 C52 P3 C41 90.4(5) . . . . ?
C53 C52 P3 Re1 -39.3(5) . . . . ?
C40 C35 P3 C52 -147.1(5) . . . . ?
C36 C35 P3 C52 42.3(6) . . . . ?
C40 C35 P3 C41 -41.2(5) . . . . ?
C36 C35 P3 C41 148.2(5) . . . . ?
C40 C35 P3 Re1 86.4(5) . . . . ?
C36 C35 P3 Re1 -84.2(5) . . . . ?
C46 C41 P3 C52 -153.7(6) . . . . ?
C42 C41 P3 C52 34.3(7) . . . . ?
C46 C41 P3 C35 98.0(6) . . . . ?
C42 C41 P3 C35 -74.0(6) . . . . ?
C46 C41 P3 Re1 -28.0(6) . . . . ?
C42 C41 P3 Re1 160.0(5) . . . . ?

_refine_diff_density_max         1.154
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.090

