# Electronic Supplementary Material (ESI) for ChemComm.
# 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. 
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data_17PF6
_database_code_depnum_ccdc_archive 'CCDC 1498858'
_audit_update_record             
;
2016-08-12 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_audit_creation_date             2016-08-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        17.PF6
_chemical_formula_moiety         'C18 H21 N5 O5 Re, F6 P, C3 H6 O'
_chemical_formula_sum            'C21 H27 F6 N5 O6 P Re'
_chemical_formula_weight         776.64
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.2779(4)
_cell_length_b                   8.9789(3)
_cell_length_c                   28.8091(10)
_cell_angle_alpha                90
_cell_angle_beta                 94.652(4)
_cell_angle_gamma                90
_cell_volume                     2649.86(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8075
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.1820
_cell_measurement_theta_min      3.6200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72490
_exptl_absorpt_correction_type   multi-scan
_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   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15252
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.838
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.3281
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4171
_reflns_number_total             4498
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4498
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0249
_refine_ls_restrained_S_all      1.168
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0227P)²+5.1406P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0585
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5-C10
 1.47 with sigma of 0.02
 N5-C10A
 1.47 with sigma of 0.02
 N5-C12A
 1.47 with sigma of 0.02
 N5-C12
 1.47 with sigma of 0.02
 C12-C11
 1.54 with sigma of 0.02
 C12A-C11
 1.54 with sigma of 0.02
 C9-C10
 1.54 with sigma of 0.02
 C9-C10A
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10) = Uanis(C10A)
Uanis(C12) = Uanis(C12A)
4. Others
 Sof(H9BD)=Sof(H9BC)=Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H9AA)=Sof(H9AB)=FVAR(1)
 Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=1-FVAR(2)
 Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C13(H13A,H13B), C11(H11A,H11B), C11(H11C,H11D), C10(H10A,H10B),
 C12(H12A,H12B), C9(H9AA,H9AB), C9(H9BD,H9BC), C7(H7A,H7B), C10A(H10C,H10D),
 C12A(H12C,H12D)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3), C2(H2)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Re3 Re 0.12051(2) 0.51371(2) 0.41587(2) 0.01631(7) Uani 1 1 d . . . . .
P1 P 0.74100(11) 0.01576(12) 0.30971(4) 0.0232(2) Uani 1 1 d . . . . .
F2 F 0.7593(3) 0.1415(3) 0.34847(10) 0.0490(8) Uani 1 1 d . . . . .
F5 F 0.5884(3) 0.0140(3) 0.31554(10) 0.0434(7) Uani 1 1 d . . . . .
F6 F 0.8931(3) 0.0175(3) 0.30322(11) 0.0440(7) Uani 1 1 d . . . . .
C1 C 0.2561(4) 0.6650(4) 0.38714(14) 0.0210(9) Uani 1 1 d . . . . .
F3 F 0.7187(3) 0.1397(4) 0.27050(11) 0.0583(9) Uani 1 1 d . . . . .
F4 F 0.7215(3) -0.1104(3) 0.27105(10) 0.0534(8) Uani 1 1 d . . . . .
O4 O -0.2099(3) 0.5183(3) 0.26532(10) 0.0292(7) Uani 1 1 d . . . . .
C8 C 0.4649(5) 0.4277(5) 0.43228(16) 0.0349(11) Uani 1 1 d . . . . .
H8A H 0.5570 0.3981 0.4301 0.042 Uiso 1 1 calc R . . . .
H8B H 0.4379 0.3881 0.4621 0.042 Uiso 1 1 calc R . . . .
N3 N 0.3865(3) 0.3537(4) 0.39468(11) 0.0225(7) Uani 1 1 d . . . . .
C5 C 0.4384(4) 0.2596(5) 0.36311(15) 0.0318(10) Uani 1 1 d . . . . .
H5 H 0.5277 0.2332 0.3622 0.038 Uiso 1 1 calc R . . . .
N4 N 0.2279(3) 0.2778(4) 0.34866(12) 0.0265(8) Uani 1 1 d . . . . .
F1 F 0.7621(3) -0.1086(3) 0.34866(10) 0.0508(8) Uani 1 1 d . . . . .
N1 N 0.3872(3) 0.6732(4) 0.39687(12) 0.0248(8) Uani 1 1 d . . . . .
O6 O 0.6003(6) 0.8431(5) 0.50032(17) 0.0869(16) Uani 1 1 d . . . . .
C13 C -0.1306(4) 0.5054(6) 0.34735(15) 0.0353(12) Uani 1 1 d . . . . .
H13A H -0.1543 0.5826 0.3697 0.042 Uiso 1 1 calc R . . . .
H13B H -0.1415 0.4077 0.3625 0.042 Uiso 1 1 calc R . . . .
C15 C -0.4556(5) 0.5144(6) 0.28505(17) 0.0416(13) Uani 1 1 d . . . . .
H15A H -0.4486 0.6033 0.2657 0.062 Uiso 1 1 calc GR . . . .
H15B H -0.5385 0.5165 0.2996 0.062 Uiso 1 1 calc GR . . . .
H15C H -0.4521 0.4251 0.2656 0.062 Uiso 1 1 calc GR . . . .
N2 N 0.2335(3) 0.7527(4) 0.34980(13) 0.0304(9) Uani 1 1 d . . . . .
C14 C -0.2295(4) 0.5134(4) 0.30543(14) 0.0247(9) Uani 1 1 d . . . . .
C6 C 0.3393(5) 0.2128(5) 0.33419(16) 0.0343(11) Uani 1 1 d . . . . .
H6 H 0.3443 0.1473 0.3085 0.041 Uiso 1 1 calc R . . . .
C19 C 0.6731(6) 0.9507(6) 0.4987(2) 0.0502(14) Uani 1 1 d . . . . .
C3 C 0.3471(5) 0.8156(5) 0.33635(17) 0.0404(12) Uani 1 1 d . . . . .
H3 H 0.3552 0.8811 0.3109 0.048 Uiso 1 1 calc R . . . .
O2 O -0.0531(3) 0.2561(4) 0.44657(11) 0.0394(8) Uani 1 1 d . . . . .
C11 C 0.1000(5) 0.2736(6) 0.3226(2) 0.0522(15) Uani 1 1 d D . . . .
H11A H 0.0346 0.2338 0.3428 0.063 Uiso 0.775(8) 1 calc R . P A 1
H11B H 0.1033 0.2064 0.2955 0.063 Uiso 0.775(8) 1 calc R . P A 1
H11C H 0.1198 0.2837 0.2897 0.063 Uiso 0.225(8) 1 calc R . P A 2
H11D H 0.0707 0.1694 0.3260 0.063 Uiso 0.225(8) 1 calc R . P A 2
C10 C 0.0024(7) 0.6903(8) 0.3256(3) 0.0377(17) Uani 0.645(8) 1 d D . P A 1
H10A H -0.0494 0.6949 0.2951 0.045 Uiso 0.645(8) 1 calc R . P A 1
H10B H -0.0479 0.7446 0.3481 0.045 Uiso 0.645(8) 1 calc R . P A 1
C12 C 0.0596(6) 0.4282(7) 0.30598(18) 0.0348(15) Uani 0.775(8) 1 d D . P A 1
H12A H 0.1364 0.4782 0.2944 0.042 Uiso 0.775(8) 1 calc R . P A 1
H12B H -0.0071 0.4183 0.2794 0.042 Uiso 0.775(8) 1 calc R . P A 1
C4 C 0.2554(4) 0.3653(4) 0.38604(13) 0.0178(8) Uani 1 1 d . . . . .
C9 C 0.1113(6) 0.7669(7) 0.3214(3) 0.076(2) Uani 1 1 d D . . . .
H9AA H 0.0863 0.8730 0.3234 0.092 Uiso 0.645(8) 1 calc R . P A 1
H9AB H 0.1332 0.7507 0.2889 0.092 Uiso 0.645(8) 1 calc R . P A 1
H9BD H 0.1247 0.8278 0.2935 0.092 Uiso 0.355(8) 1 calc R . P A 2
H9BC H 0.0463 0.8180 0.3393 0.092 Uiso 0.355(8) 1 calc R . P A 2
N5 N 0.0074(3) 0.5232(4) 0.34093(12) 0.0264(8) Uani 1 1 d D . . . .
C16 C 0.2013(4) 0.5075(4) 0.47731(14) 0.0238(9) Uani 1 1 d . . . . .
C17 C 0.0094(4) 0.3537(5) 0.43503(12) 0.0235(9) Uani 1 1 d . . . . .
C2 C 0.4432(4) 0.7662(5) 0.36621(16) 0.0331(11) Uani 1 1 d . . . . .
H2 H 0.5332 0.7906 0.3663 0.040 Uiso 1 1 calc R . . . .
C7 C 0.4603(5) 0.5949(5) 0.43477(18) 0.0430(13) Uani 1 1 d . . . . .
H7A H 0.4228 0.6226 0.4642 0.052 Uiso 1 1 calc R . . . .
H7B H 0.5512 0.6323 0.4368 0.052 Uiso 1 1 calc R . . . .
C21 C 0.6762(7) 1.0346(8) 0.4555(2) 0.073(2) Uani 1 1 d . . . . .
H21A H 0.7597 1.0176 0.4422 0.110 Uiso 1 1 calc GR . . . .
H21B H 0.6662 1.1410 0.4619 0.110 Uiso 1 1 calc GR . . . .
H21C H 0.6046 1.0016 0.4333 0.110 Uiso 1 1 calc GR . . . .
C20 C 0.7606(8) 0.9924(6) 0.5392(2) 0.0689(19) Uani 1 1 d . . . . .
H20A H 0.7487 0.9234 0.5648 0.103 Uiso 1 1 calc GR . . . .
H20B H 0.7405 1.0940 0.5488 0.103 Uiso 1 1 calc GR . . . .
H20C H 0.8512 0.9878 0.5310 0.103 Uiso 1 1 calc GR . . . .
O5 O -0.3479(3) 0.5117(3) 0.32112(10) 0.0338(8) Uani 1 1 d . . . . .
O1 O 0.2455(3) 0.5039(4) 0.51558(10) 0.0385(8) Uani 1 1 d . . . . .
O3 O -0.0590(3) 0.7598(4) 0.45091(11) 0.0389(8) Uani 1 1 d . . . . .
C18 C 0.0059(4) 0.6684(5) 0.43763(14) 0.0251(9) Uani 1 1 d . . . . .
C10A C 0.0595(13) 0.6120(13) 0.3061(4) 0.0377(17) Uani 0.355(8) 1 d D . P A 2
H10C H -0.0093 0.6256 0.2804 0.045 Uiso 0.355(8) 1 calc R . P A 2
H10D H 0.1317 0.5560 0.2935 0.045 Uiso 0.355(8) 1 calc R . P A 2
C12A C -0.0113(16) 0.3562(18) 0.3254(7) 0.0348(15) Uani 0.225(8) 1 d D . P A 2
H12C H -0.0657 0.3063 0.3476 0.042 Uiso 0.225(8) 1 calc R . P A 2
H12D H -0.0609 0.3546 0.2945 0.042 Uiso 0.225(8) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re3 C1 2.159(4) . ?
Re3 C4 2.152(4) . ?
Re3 N5 2.369(3) . ?
Re3 C16 1.894(4) . ?
Re3 C17 1.943(4) . ?
Re3 C18 1.957(4) . ?
P1 F2 1.588(3) . ?
P1 F5 1.591(3) . ?
P1 F6 1.589(3) . ?
P1 F3 1.589(3) . ?
P1 F4 1.590(3) . ?
P1 F1 1.585(3) . ?
C1 N1 1.355(5) . ?
C1 N2 1.338(5) . ?
O4 C14 1.190(5) . ?
C8 N3 1.456(5) . ?
C8 C7 1.504(7) . ?
N3 C5 1.380(5) . ?
N3 C4 1.354(5) . ?
C5 C6 1.330(6) . ?
N4 C6 1.380(5) . ?
N4 C11 1.460(6) . ?
N4 C4 1.344(5) . ?
N1 C2 1.376(5) . ?
N1 C7 1.455(5) . ?
O6 C19 1.226(7) . ?
C13 C14 1.516(6) . ?
C13 N5 1.454(6) . ?
C15 O5 1.455(5) . ?
N2 C3 1.381(6) . ?
N2 C9 1.449(6) . ?
C14 O5 1.332(5) . ?
C19 C21 1.457(8) . ?
C19 C20 1.463(8) . ?
C3 C2 1.332(7) . ?
O2 C17 1.152(5) . ?
C11 C12 1.516(8) . ?
C11 C12A 1.371(14) . ?
C10 C9 1.327(9) . ?
C10 N5 1.564(7) . ?
C12 N5 1.455(6) . ?
C9 C10A 1.540(12) . ?
N5 C10A 1.419(12) . ?
N5 C12A 1.573(15) . ?
C16 O1 1.158(5) . ?
O3 C18 1.142(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
C1 Re3 N5 84.96(14) . . ?
C4 Re3 C1 77.27(15) . . ?
C4 Re3 N5 86.73(13) . . ?
C16 Re3 C1 97.41(16) . . ?
C16 Re3 C4 96.15(16) . . ?
C16 Re3 N5 176.60(15) . . ?
C16 Re3 C17 86.33(16) . . ?
C16 Re3 C18 87.20(17) . . ?
C17 Re3 C1 170.71(15) . . ?
C17 Re3 C4 93.92(16) . . ?
C17 Re3 N5 91.69(14) . . ?
C17 Re3 C18 92.91(18) . . ?
C18 Re3 C1 95.75(16) . . ?
C18 Re3 C4 172.57(16) . . ?
C18 Re3 N5 90.15(15) . . ?
F2 P1 F5 89.69(16) . . ?
F2 P1 F6 90.80(16) . . ?
F2 P1 F3 90.22(18) . . ?
F2 P1 F4 179.53(18) . . ?
F6 P1 F5 179.30(17) . . ?
F6 P1 F4 89.66(16) . . ?
F3 P1 F5 89.72(16) . . ?
F3 P1 F6 89.77(16) . . ?
F3 P1 F4 89.90(19) . . ?
F4 P1 F5 89.86(16) . . ?
F1 P1 F2 90.10(18) . . ?
F1 P1 F5 89.86(16) . . ?
F1 P1 F6 90.64(16) . . ?
F1 P1 F3 179.5(2) . . ?
F1 P1 F4 89.77(18) . . ?
N1 C1 Re3 128.1(3) . . ?
N2 C1 Re3 127.1(3) . . ?
N2 C1 N1 103.8(3) . . ?
N3 C8 C7 118.2(4) . . ?
C5 N3 C8 123.3(4) . . ?
C4 N3 C8 125.7(4) . . ?
C4 N3 C5 110.9(3) . . ?
C6 C5 N3 106.8(4) . . ?
C6 N4 C11 124.6(4) . . ?
C4 N4 C6 111.3(3) . . ?
C4 N4 C11 123.3(4) . . ?
C1 N1 C2 111.2(3) . . ?
C1 N1 C7 125.0(4) . . ?
C2 N1 C7 123.9(4) . . ?
N5 C13 C14 119.4(4) . . ?
C1 N2 C3 111.8(4) . . ?
C1 N2 C9 126.3(4) . . ?
C3 N2 C9 121.3(4) . . ?
O4 C14 C13 128.3(4) . . ?
O4 C14 O5 124.1(4) . . ?
O5 C14 C13 107.5(3) . . ?
C5 C6 N4 106.8(4) . . ?
O6 C19 C21 119.8(6) . . ?
O6 C19 C20 120.6(6) . . ?
C21 C19 C20 119.6(6) . . ?
C2 C3 N2 106.4(4) . . ?
N4 C11 C12 110.5(4) . . ?
C12A C11 N4 132.6(8) . . ?
C9 C10 N5 121.0(6) . . ?
N5 C12 C11 115.2(5) . . ?
N3 C4 Re3 129.6(3) . . ?
N4 C4 Re3 125.5(3) . . ?
N4 C4 N3 104.1(3) . . ?
N2 C9 C10A 110.2(6) . . ?
C10 C9 N2 127.0(6) . . ?
C13 N5 Re3 107.0(2) . . ?
C13 N5 C10 97.6(4) . . ?
C13 N5 C12 116.2(4) . . ?
C13 N5 C12A 80.4(7) . . ?
C10 N5 Re3 107.1(3) . . ?
C12 N5 Re3 115.3(3) . . ?
C12 N5 C10 111.9(5) . . ?
C10A N5 Re3 118.6(5) . . ?
C10A N5 C13 125.4(6) . . ?
C10A N5 C12A 112.3(9) . . ?
C12A N5 Re3 105.3(7) . . ?
O1 C16 Re3 177.1(4) . . ?
O2 C17 Re3 177.9(4) . . ?
C3 C2 N1 106.8(4) . . ?
N1 C7 C8 117.6(4) . . ?
C14 O5 C15 114.8(3) . . ?
O3 C18 Re3 178.6(4) . . ?
N5 C10A C9 116.6(9) . . ?
C11 C12A N5 116.7(12) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_16PF6
_database_code_depnum_ccdc_archive 'CCDC 1498859'
_audit_update_record             
;
2016-08-12 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_audit_creation_date             2016-08-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        16.PF6
_chemical_formula_moiety         'C32 H32 N8 O4 Re S, F6 P'
_chemical_formula_sum            'C32 H32 F6 N8 O4 P Re S'
_chemical_formula_weight         955.88
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7659(3)
_cell_length_b                   12.9987(7)
_cell_length_c                   16.3263(11)
_cell_angle_alpha                68.155(6)
_cell_angle_beta                 76.597(4)
_cell_angle_gamma                81.414(4)
_cell_volume                     1675.61(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9121
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.3320
_cell_measurement_theta_min      4.7040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62808
_exptl_absorpt_correction_type   multi-scan
_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   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15862
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.978
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.3281
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6318
_reflns_number_total             6840
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.301
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         6840
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0264
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0317P)²+0.9905P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0645
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9A-C10
 1.54 with sigma of 0.02
 C9-C10
 1.54 with sigma of 0.02
 N2-C9
 1.47 with sigma of 0.02
 N2-C9A
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C9A)
4. Others
 Sof(H10C)=Sof(H10D)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(1)
 Sof(H10A)=Sof(H10B)=Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C7(H7A,H7B), C8(H8A,H8B), C11(H11A,H11B), C10(H10A,H10B),
 C10(H10C,H10D), C9(H9A,H9B), C9A(H9AA,H9AB), C12(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), N6(H6A), C20(H20), C26(H26), C2(H2), C17(H17), C3(H3),
 C16(H16), C24(H24), C23(H23), C27(H27)
5.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Re1 Re 0.03824(2) 0.74764(2) 1.07393(2) 0.01830(5) Uani 1 1 d . . . . .
S1 S 0.52413(11) 0.33541(8) 0.64090(7) 0.0311(2) Uani 1 1 d . . . . .
P1 P 0.18183(10) 0.14884(8) 0.24014(7) 0.0280(2) Uani 1 1 d . . . . .
F5 F 0.3521(3) 0.1864(2) 0.22880(18) 0.0488(7) Uani 1 1 d . . . . .
F4 F 0.2235(4) 0.1498(5) 0.1423(2) 0.1198(19) Uani 1 1 d . . . . .
F2 F 0.1372(4) 0.1533(3) 0.3374(2) 0.0855(11) Uani 1 1 d . . . . .
F6 F 0.0100(3) 0.1166(2) 0.2481(2) 0.0585(8) Uani 1 1 d . . . . .
O3 O -0.2183(3) 0.6258(2) 1.0522(2) 0.0404(7) Uani 1 1 d . . . . .
O4 O 0.4063(3) 0.5897(2) 0.83871(18) 0.0321(6) Uani 1 1 d . . . . .
F3 F 0.1228(3) 0.2742(3) 0.2039(3) 0.0970(14) Uani 1 1 d . . . . .
C13 C 0.1626(4) 0.6603(3) 0.9132(3) 0.0308(8) Uani 1 1 d . . . . .
H13A H 0.1006 0.7287 0.8833 0.037 Uiso 1 1 calc R . . . .
H13B H 0.0874 0.6027 0.9488 0.037 Uiso 1 1 calc R . . . .
O1 O -0.2330(3) 0.8439(3) 1.1843(2) 0.0544(9) Uani 1 1 d . . . . .
N1 N 0.2426(3) 0.8314(2) 1.1705(2) 0.0226(6) Uani 1 1 d . . . . .
C6 C 0.2567(4) 0.4620(3) 1.2584(3) 0.0279(8) Uani 1 1 d . . . . .
H6 H 0.3181 0.3932 1.2707 0.033 Uiso 1 1 calc R . . . .
N5 N 0.2363(3) 0.6836(2) 0.9772(2) 0.0223(6) Uani 1 1 d . . . . .
C5 C 0.2121(4) 0.5218(3) 1.3124(3) 0.0282(8) Uani 1 1 d . . . . .
H5 H 0.2343 0.5031 1.3707 0.034 Uiso 1 1 calc R . . . .
N6 N 0.1867(3) 0.6221(3) 0.7795(2) 0.0289(7) Uani 1 1 d . . . . .
H6A H 0.0937 0.6586 0.7808 0.035 Uiso 1 1 calc R . . . .
N2 N 0.3735(3) 0.8364(3) 1.0415(2) 0.0281(7) Uani 1 1 d D . . . .
N7 N 0.3317(3) 0.4053(2) 0.5296(2) 0.0260(7) Uani 1 1 d . . . . .
N4 N 0.1965(3) 0.5194(2) 1.1818(2) 0.0226(6) Uani 1 1 d . . . . .
C29 C 0.8333(5) -0.0737(4) 0.4314(3) 0.0414(10) Uani 1 1 d . . . . .
H29A H 0.8417 -0.1365 0.4108 0.062 Uiso 1 1 calc GR . . . .
H29B H 0.8104 -0.1005 0.4972 0.062 Uiso 1 1 calc GR . . . .
H29C H 0.9328 -0.0376 0.4091 0.062 Uiso 1 1 calc GR . . . .
N3 N 0.1271(3) 0.6164(2) 1.2667(2) 0.0246(6) Uani 1 1 d . . . . .
O2 O -0.0336(4) 0.9614(2) 0.9185(2) 0.0524(9) Uani 1 1 d . . . . .
C28 C 0.6613(5) 0.0026(4) 0.3193(3) 0.0451(11) Uani 1 1 d . . . . .
H28A H 0.7065 0.0634 0.2659 0.068 Uiso 1 1 calc GR . . . .
H28B H 0.5464 0.0110 0.3272 0.068 Uiso 1 1 calc GR . . . .
H28C H 0.6996 -0.0686 0.3116 0.068 Uiso 1 1 calc GR . . . .
C0AA C 0.2298(4) 0.8155(3) 1.0949(2) 0.0205(7) Uani 1 1 d . . . . .
C20 C 0.3548(4) 0.4894(3) 0.7169(3) 0.0268(8) Uani 1 1 d . . . . .
H20 H 0.4185 0.4691 0.7611 0.032 Uiso 1 1 calc R . . . .
N8 N 0.7074(4) 0.0058(3) 0.3972(2) 0.0352(8) Uani 1 1 d . . . . .
C26 C 0.7089(5) 0.0995(4) 0.5000(3) 0.0399(10) Uani 1 1 d . . . . .
H26 H 0.7940 0.0505 0.5219 0.048 Uiso 1 1 calc R . . . .
C7 C 0.1167(4) 0.8212(3) 1.2483(2) 0.0275(8) Uani 1 1 d . . . . .
H7A H 0.0257 0.8713 1.2277 0.033 Uiso 1 1 calc R . . . .
H7B H 0.1528 0.8482 1.2895 0.033 Uiso 1 1 calc R . . . .
C2 C 0.3896(4) 0.8629(3) 1.1634(3) 0.0307(9) Uani 1 1 d . . . . .
H2 H 0.4253 0.8799 1.2073 0.037 Uiso 1 1 calc R . . . .
C17 C 0.1701(4) 0.5487(3) 0.5853(3) 0.0295(8) Uani 1 1 d . . . . .
H17 H 0.1071 0.5701 0.5406 0.035 Uiso 1 1 calc R . . . .
C30 C -0.1277(4) 0.8060(3) 1.1454(3) 0.0307(9) Uani 1 1 d . . . . .
C32 C -0.1214(4) 0.6702(3) 1.0606(2) 0.0246(7) Uani 1 1 d . . . . .
C15 C 0.2328(4) 0.5699(3) 0.7141(2) 0.0250(7) Uani 1 1 d . . . . .
C18 C 0.2908(4) 0.4656(3) 0.5872(2) 0.0237(7) Uani 1 1 d . . . . .
C8 C 0.0597(5) 0.7042(3) 1.3023(3) 0.0324(9) Uani 1 1 d . . . . .
H8A H 0.0814 0.6817 1.3637 0.039 Uiso 1 1 calc R . . . .
H8B H -0.0558 0.7089 1.3080 0.039 Uiso 1 1 calc R . . . .
C3 C 0.4716(4) 0.8650(3) 1.0841(3) 0.0338(9) Uani 1 1 d . . . . .
H3 H 0.5780 0.8828 1.0606 0.041 Uiso 1 1 calc R . . . .
C31 C -0.0057(4) 0.8800(3) 0.9735(3) 0.0277(8) Uani 1 1 d . . . . .
C16 C 0.1422(4) 0.5995(3) 0.6472(3) 0.0289(8) Uani 1 1 d . . . . .
H16 H 0.0595 0.6562 0.6452 0.035 Uiso 1 1 calc R . . . .
C11 C 0.2397(4) 0.4950(3) 1.0986(3) 0.0291(8) Uani 1 1 d . . . . .
H11A H 0.1434 0.4887 1.0795 0.035 Uiso 1 1 calc R . . . .
H11B H 0.3026 0.4229 1.1095 0.035 Uiso 1 1 calc R . . . .
C14 C 0.2692(4) 0.6220(3) 0.8396(2) 0.0257(8) Uani 1 1 d . . . . .
C21 C 0.4500(4) 0.3336(3) 0.5500(2) 0.0242(7) Uani 1 1 d . . . . .
C4 C 0.1160(4) 0.6163(3) 1.1853(2) 0.0211(7) Uani 1 1 d . . . . .
C19 C 0.3813(4) 0.4391(3) 0.6532(2) 0.0244(7) Uani 1 1 d . . . . .
C25 C 0.6512(4) 0.0896(3) 0.4299(3) 0.0280(8) Uani 1 1 d . . . . .
C24 C 0.5313(4) 0.1679(3) 0.3977(3) 0.0319(9) Uani 1 1 d . . . . .
H24 H 0.4921 0.1662 0.3486 0.038 Uiso 1 1 calc R . . . .
C23 C 0.4689(4) 0.2473(3) 0.4354(2) 0.0300(8) Uani 1 1 d . . . . .
H23 H 0.3872 0.2989 0.4119 0.036 Uiso 1 1 calc R . . . .
C27 C 0.6448(5) 0.1783(4) 0.5371(3) 0.0380(10) Uani 1 1 d . . . . .
H27 H 0.6854 0.1816 0.5851 0.046 Uiso 1 1 calc R . . . .
C22 C 0.5218(4) 0.2541(3) 0.5070(3) 0.0255(8) Uani 1 1 d . . . . .
C10 C 0.3367(5) 0.7791(4) 0.9176(3) 0.0439(10) Uani 1 1 d D . . . .
H10A H 0.4029 0.7580 0.8675 0.053 Uiso 0.851(10) 1 calc R . P A 1
H10B H 0.2658 0.8438 0.8910 0.053 Uiso 0.851(10) 1 calc R . P A 1
H10C H 0.4386 0.7441 0.8961 0.053 Uiso 0.149(10) 1 calc R . P A 2
H10D H 0.2873 0.8166 0.8642 0.053 Uiso 0.149(10) 1 calc R . P A 2
C9 C 0.4390(5) 0.8145(4) 0.9591(3) 0.0336(13) Uani 0.851(10) 1 d D . P A 1
H9A H 0.5266 0.7566 0.9712 0.040 Uiso 0.851(10) 1 calc R . P A 1
H9B H 0.4854 0.8830 0.9141 0.040 Uiso 0.851(10) 1 calc R . P A 1
F1 F 0.2381(4) 0.0245(3) 0.2796(3) 0.1054(15) Uani 1 1 d . . . . .
C9A C 0.378(4) 0.8701(19) 0.9415(12) 0.0336(13) Uani 0.149(10) 1 d D . P A 2
H9AA H 0.3025 0.9354 0.9227 0.040 Uiso 0.149(10) 1 calc R . P A 2
H9AB H 0.4840 0.8923 0.9080 0.040 Uiso 0.149(10) 1 calc R . P A 2
C12 C 0.3342(4) 0.5855(3) 1.0246(3) 0.0326(9) Uani 1 1 d . . . . .
H12A H 0.4064 0.6103 1.0510 0.039 Uiso 1 1 calc R . . . .
H12B H 0.3992 0.5539 0.9802 0.039 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
Re1 N5 2.341(3) . ?
Re1 C0AA 2.156(3) . ?
Re1 C30 1.896(4) . ?
Re1 C32 1.935(3) . ?
Re1 C31 1.948(4) . ?
Re1 C4 2.146(3) . ?
S1 C21 1.762(4) . ?
S1 C19 1.733(4) . ?
P1 F5 1.589(2) . ?
P1 F4 1.549(3) . ?
P1 F2 1.565(3) . ?
P1 F6 1.587(2) . ?
P1 F3 1.564(3) . ?
P1 F1 1.551(3) . ?
O3 C32 1.154(4) . ?
O4 C14 1.211(4) . ?
C13 N5 1.485(4) . ?
C13 C14 1.532(5) . ?
O1 C30 1.151(5) . ?
N1 C0AA 1.355(4) . ?
N1 C7 1.456(5) . ?
N1 C2 1.377(4) . ?
C6 C5 1.339(5) . ?
C6 N4 1.377(4) . ?
N5 C10 1.514(5) . ?
N5 C12 1.486(4) . ?
C5 N3 1.388(4) . ?
N6 C15 1.422(5) . ?
N6 C14 1.348(5) . ?
N2 C0AA 1.356(4) . ?
N2 C3 1.389(5) . ?
N2 C9 1.449(5) . ?
N2 C9A 1.518(17) . ?
N7 C18 1.391(5) . ?
N7 C21 1.302(4) . ?
N4 C11 1.460(5) . ?
N4 C4 1.362(4) . ?
C29 N8 1.453(5) . ?
N3 C8 1.458(5) . ?
N3 C4 1.355(5) . ?
O2 C31 1.141(4) . ?
C28 N8 1.438(5) . ?
C20 C15 1.376(5) . ?
C20 C19 1.382(5) . ?
N8 C25 1.365(5) . ?
C26 C25 1.407(5) . ?
C26 C27 1.365(6) . ?
C7 C8 1.538(5) . ?
C2 C3 1.319(6) . ?
C17 C18 1.392(5) . ?
C17 C16 1.361(5) . ?
C15 C16 1.402(5) . ?
C18 C19 1.396(5) . ?
C11 C12 1.516(5) . ?
C21 C22 1.448(5) . ?
C25 C24 1.398(5) . ?
C24 C23 1.376(5) . ?
C23 C22 1.388(5) . ?
C27 C22 1.394(5) . ?
C10 C9 1.453(6) . ?
C10 C9A 1.489(17) . ?

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
C0AA Re1 N5 83.65(11) . . ?
C30 Re1 N5 176.14(13) . . ?
C30 Re1 C0AA 97.83(14) . . ?
C30 Re1 C32 85.69(15) . . ?
C30 Re1 C31 85.82(17) . . ?
C30 Re1 C4 95.29(15) . . ?
C32 Re1 N5 93.18(13) . . ?
C32 Re1 C0AA 173.46(13) . . ?
C32 Re1 C31 91.69(15) . . ?
C32 Re1 C4 97.54(14) . . ?
C31 Re1 N5 90.52(13) . . ?
C31 Re1 C0AA 94.05(14) . . ?
C31 Re1 C4 170.76(13) . . ?
C4 Re1 N5 88.52(12) . . ?
C4 Re1 C0AA 76.71(12) . . ?
C19 S1 C21 89.80(17) . . ?
F4 P1 F5 89.60(16) . . ?
F4 P1 F2 177.5(3) . . ?
F4 P1 F6 89.30(16) . . ?
F4 P1 F3 89.1(3) . . ?
F4 P1 F1 92.9(3) . . ?
F2 P1 F5 90.33(16) . . ?
F2 P1 F6 90.66(17) . . ?
F6 P1 F5 177.39(16) . . ?
F3 P1 F5 88.72(15) . . ?
F3 P1 F2 88.4(2) . . ?
F3 P1 F6 88.90(16) . . ?
F1 P1 F5 91.54(17) . . ?
F1 P1 F2 89.6(2) . . ?
F1 P1 F6 90.88(18) . . ?
F1 P1 F3 177.9(3) . . ?
N5 C13 C14 118.6(3) . . ?
C0AA N1 C7 125.2(3) . . ?
C0AA N1 C2 111.3(3) . . ?
C2 N1 C7 123.5(3) . . ?
C5 C6 N4 106.8(3) . . ?
C13 N5 Re1 108.4(2) . . ?
C13 N5 C10 103.5(3) . . ?
C13 N5 C12 111.5(3) . . ?
C10 N5 Re1 108.1(2) . . ?
C12 N5 Re1 113.7(2) . . ?
C12 N5 C10 111.0(3) . . ?
C6 C5 N3 106.6(3) . . ?
C14 N6 C15 127.4(3) . . ?
C0AA N2 C3 110.5(3) . . ?
C0AA N2 C9 129.0(3) . . ?
C0AA N2 C9A 115.3(12) . . ?
C3 N2 C9 119.4(3) . . ?
C3 N2 C9A 128.7(9) . . ?
C21 N7 C18 111.0(3) . . ?
C6 N4 C11 125.1(3) . . ?
C4 N4 C6 111.6(3) . . ?
C4 N4 C11 122.0(3) . . ?
C5 N3 C8 123.8(3) . . ?
C4 N3 C5 111.4(3) . . ?
C4 N3 C8 124.9(3) . . ?
N1 C0AA Re1 127.5(2) . . ?
N1 C0AA N2 103.9(3) . . ?
N2 C0AA Re1 128.0(3) . . ?
C15 C20 C19 117.6(3) . . ?
C28 N8 C29 117.2(3) . . ?
C25 N8 C29 121.1(3) . . ?
C25 N8 C28 121.1(3) . . ?
C27 C26 C25 121.2(4) . . ?
N1 C7 C8 116.4(3) . . ?
C3 C2 N1 107.0(3) . . ?
C16 C17 C18 120.0(3) . . ?
O1 C30 Re1 175.8(3) . . ?
O3 C32 Re1 178.8(3) . . ?
C20 C15 N6 123.0(3) . . ?
C20 C15 C16 120.0(3) . . ?
C16 C15 N6 117.0(3) . . ?
N7 C18 C17 126.6(3) . . ?
N7 C18 C19 115.8(3) . . ?
C17 C18 C19 117.5(3) . . ?
N3 C8 C7 117.1(3) . . ?
C2 C3 N2 107.2(3) . . ?
O2 C31 Re1 175.5(3) . . ?
C17 C16 C15 121.4(3) . . ?
N4 C11 C12 110.9(3) . . ?
O4 C14 C13 124.6(3) . . ?
O4 C14 N6 124.6(3) . . ?
N6 C14 C13 110.7(3) . . ?
N7 C21 S1 114.6(3) . . ?
N7 C21 C22 126.8(3) . . ?
C22 C21 S1 118.6(3) . . ?
N4 C4 Re1 125.4(3) . . ?
N3 C4 Re1 129.8(2) . . ?
N3 C4 N4 103.6(3) . . ?
C20 C19 S1 127.9(3) . . ?
C20 C19 C18 123.4(3) . . ?
C18 C19 S1 108.8(3) . . ?
N8 C25 C26 121.2(3) . . ?
N8 C25 C24 122.3(3) . . ?
C24 C25 C26 116.5(3) . . ?
C23 C24 C25 121.5(3) . . ?
C24 C23 C22 121.9(3) . . ?
C26 C27 C22 122.3(4) . . ?
C23 C22 C21 121.8(3) . . ?
C23 C22 C27 116.6(3) . . ?
C27 C22 C21 121.6(3) . . ?
C9 C10 N5 117.3(4) . . ?
C9A C10 N5 127.6(9) . . ?
N2 C9 C10 118.9(4) . . ?
C10 C9A N2 112.5(13) . . ?
N5 C12 C11 113.8(3) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_15PF6
_database_code_depnum_ccdc_archive 'CCDC 1498857'
_audit_update_record             
;
2016-08-12 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_audit_creation_date             2016-08-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        15.PF6
_chemical_formula_moiety         'C33 H35 N7 O4 Re, F6 P, C3 H6 O'
_chemical_formula_sum            'C36 H41 F6 N7 O5 P Re'
_chemical_formula_weight         982.93
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3606(5)
_cell_length_b                   12.7288(4)
_cell_length_c                   14.7762(6)
_cell_angle_alpha                108.108(3)
_cell_angle_beta                 103.558(4)
_cell_angle_gamma                100.145(3)
_cell_volume                     1901.26(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9356
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.0140
_cell_measurement_theta_min      3.8050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.320
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90057
_exptl_absorpt_correction_type   multi-scan
_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   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         2.793
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.3281
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5993
_reflns_number_total             6461
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         6461
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0238
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0241P)²+0.9499P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0546
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-F5A = P1-F5 = P1-F4A = P1-F4 = P1-F3 = P1-F6A = P1-F6 = P1-F1 = P1-F2
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F6A)
Uanis(F3) = Uanis(F3A)
Uanis(F4) = Uanis(F4A)
Uanis(F5) = Uanis(F5A)
4. Others
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 N6(H6), C2(H2), C3(H3), C5(H5), C6(H6A), C16(H16), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28)
5.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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
Re1 Re 0.57143(2) -0.26175(2) 0.68793(2) 0.02327(5) Uani 1 1 d . . . . .
O1 O 0.6495(3) -0.4189(2) 0.5228(2) 0.0492(7) Uani 1 1 d . . . . .
O2 O 0.3188(3) -0.3371(2) 0.51804(19) 0.0402(6) Uani 1 1 d . . . . .
O3 O 0.6929(3) -0.0816(2) 0.6132(2) 0.0434(7) Uani 1 1 d . . . . .
O4 O 0.4144(3) 0.0802(2) 0.88510(17) 0.0373(6) Uani 1 1 d . . . . .
N1 N 0.5603(3) -0.4623(2) 0.7728(2) 0.0314(7) Uani 1 1 d . . . . .
N2 N 0.4563(3) -0.3524(2) 0.8373(2) 0.0289(6) Uani 1 1 d . . . . .
N3 N 0.7965(3) -0.3115(2) 0.8272(2) 0.0311(7) Uani 1 1 d . . . . .
N4 N 0.7878(3) -0.1381(2) 0.8893(2) 0.0297(6) Uani 1 1 d . . . . .
N5 N 0.5099(2) -0.1254(2) 0.80261(19) 0.0232(6) Uani 1 1 d . . . . .
N6 N 0.3604(3) 0.0842(2) 0.7277(2) 0.0299(6) Uani 1 1 d . . . . .
H6 H 0.3577 0.0447 0.6663 0.036 Uiso 1 1 calc R . . . .
N7 N -0.0017(4) 0.9174(3) 0.6774(2) 0.0497(9) Uani 1 1 d . . . . .
C1 C 0.5143(3) -0.3724(3) 0.7658(2) 0.0265(7) Uani 1 1 d . . . . .
C2 C 0.5329(4) -0.4959(3) 0.8472(3) 0.0405(9) Uani 1 1 d . . . . .
H2 H 0.5559 -0.5562 0.8659 0.049 Uiso 1 1 calc R . . . .
C3 C 0.4682(4) -0.4278(3) 0.8879(3) 0.0390(9) Uani 1 1 d . . . . .
H3 H 0.4361 -0.4300 0.9413 0.047 Uiso 1 1 calc R . . . .
C4 C 0.7364(3) -0.2343(3) 0.8056(2) 0.0271(7) Uani 1 1 d . . . . .
C5 C 0.8811(4) -0.2644(4) 0.9221(3) 0.0422(9) Uani 1 1 d . . . . .
H5 H 0.9332 -0.3017 0.9539 0.051 Uiso 1 1 calc R . . . .
C6 C 0.8759(4) -0.1561(4) 0.9612(3) 0.0431(9) Uani 1 1 d . . . . .
H6A H 0.9236 -0.1018 1.0261 0.052 Uiso 1 1 calc R . . . .
C7 C 0.6431(4) -0.5067(3) 0.7181(3) 0.0376(9) Uani 1 1 d . . . . .
H7A H 0.6079 -0.5168 0.6470 0.045 Uiso 1 1 calc R . . . .
H7B H 0.6451 -0.5833 0.7205 0.045 Uiso 1 1 calc R . . . .
C8 C 0.7783(4) -0.4293(3) 0.7589(3) 0.0385(9) Uani 1 1 d . . . . .
H8A H 0.8329 -0.4659 0.7946 0.046 Uiso 1 1 calc R . . . .
H8B H 0.8071 -0.4253 0.7015 0.046 Uiso 1 1 calc R . . . .
C9 C 0.3947(3) -0.2616(3) 0.8689(3) 0.0291(7) Uani 1 1 d . . . . .
H9A H 0.4397 -0.2142 0.9403 0.035 Uiso 1 1 calc R . . . .
H9B H 0.3079 -0.2981 0.8643 0.035 Uiso 1 1 calc R . . . .
C10 C 0.3882(3) -0.1832(3) 0.8110(2) 0.0280(7) Uani 1 1 d . . . . .
H10A H 0.3303 -0.2283 0.7425 0.034 Uiso 1 1 calc R . . . .
H10B H 0.3503 -0.1230 0.8427 0.034 Uiso 1 1 calc R . . . .
C11 C 0.7398(3) -0.0363(3) 0.9031(3) 0.0337(8) Uani 1 1 d . . . . .
H11A H 0.7448 -0.0085 0.8482 0.040 Uiso 1 1 calc R . . . .
H11B H 0.7931 0.0254 0.9671 0.040 Uiso 1 1 calc R . . . .
C12 C 0.6050(3) -0.0623(3) 0.9043(2) 0.0287(7) Uani 1 1 d . . . . .
H12A H 0.5964 -0.1087 0.9463 0.034 Uiso 1 1 calc R . . . .
H12B H 0.5860 0.0109 0.9359 0.034 Uiso 1 1 calc R . . . .
C13 C 0.4824(3) -0.0415(3) 0.7539(2) 0.0278(7) Uani 1 1 d . . . . .
H13A H 0.4312 -0.0862 0.6833 0.033 Uiso 1 1 calc R . . . .
H13B H 0.5634 0.0017 0.7530 0.033 Uiso 1 1 calc R . . . .
C14 C 0.4152(3) 0.0463(3) 0.7983(2) 0.0274(7) Uani 1 1 d . . . . .
C15 C 0.3065(3) 0.1780(3) 0.7373(2) 0.0288(7) Uani 1 1 d . . . . .
C16 C 0.2840(4) 0.2119(3) 0.6549(3) 0.0371(9) Uani 1 1 d . . . . .
H16 H 0.3055 0.1725 0.5977 0.045 Uiso 1 1 calc R . . . .
C17 C 0.2314(4) 0.3006(3) 0.6552(3) 0.0386(9) Uani 1 1 d . . . . .
H17 H 0.2170 0.3219 0.5982 0.046 Uiso 1 1 calc R . . . .
C18 C 0.1986(3) 0.3606(3) 0.7380(3) 0.0316(8) Uani 1 1 d . . . . .
C19 C 0.2208(4) 0.3256(3) 0.8196(3) 0.0335(8) Uani 1 1 d . . . . .
H19 H 0.1980 0.3640 0.8765 0.040 Uiso 1 1 calc R . . . .
C20 C 0.2755(3) 0.2359(3) 0.8202(3) 0.0317(8) Uani 1 1 d . . . . .
H20 H 0.2913 0.2149 0.8773 0.038 Uiso 1 1 calc R . . . .
C21 C 0.1470(3) 0.4597(3) 0.7421(3) 0.0346(8) Uani 1 1 d . . . . .
H21 H 0.1236 0.4940 0.7997 0.041 Uiso 1 1 calc R . . . .
C22 C 0.1305(3) 0.5054(3) 0.6719(3) 0.0329(8) Uani 1 1 d . . . . .
H22 H 0.1468 0.4656 0.6121 0.040 Uiso 1 1 calc R . . . .
C23 C 0.0904(3) 0.6092(3) 0.6754(3) 0.0305(8) Uani 1 1 d . . . . .
C24 C 0.0762(3) 0.6415(3) 0.5919(3) 0.0334(8) Uani 1 1 d . . . . .
H24 H 0.0884 0.5929 0.5334 0.040 Uiso 1 1 calc R . . . .
C25 C 0.0454(4) 0.7414(3) 0.5920(3) 0.0358(8) Uani 1 1 d . . . . .
H25 H 0.0356 0.7595 0.5334 0.043 Uiso 1 1 calc R . . . .
C26 C 0.0281(3) 0.8168(3) 0.6765(3) 0.0343(8) Uani 1 1 d . . . . .
C27 C 0.0424(3) 0.7847(3) 0.7603(3) 0.0326(8) Uani 1 1 d . . . . .
H27 H 0.0319 0.8338 0.8193 0.039 Uiso 1 1 calc R . . . .
C28 C 0.0713(3) 0.6834(3) 0.7590(3) 0.0304(8) Uani 1 1 d . . . . .
H28 H 0.0785 0.6639 0.8167 0.037 Uiso 1 1 calc R . . . .
C29 C -0.0007(5) 0.9538(3) 0.5937(3) 0.0514(11) Uani 1 1 d . . . . .
H29A H 0.0823 0.9601 0.5840 0.077 Uiso 1 1 calc GR . . . .
H29B H -0.0190 1.0286 0.6077 0.077 Uiso 1 1 calc GR . . . .
H29C H -0.0647 0.8973 0.5329 0.077 Uiso 1 1 calc GR . . . .
C30 C 0.0012(5) 1.0007(3) 0.7686(3) 0.0513(11) Uani 1 1 d . . . . .
H30A H -0.0576 0.9664 0.7972 0.077 Uiso 1 1 calc GR . . . .
H30B H -0.0233 1.0660 0.7556 0.077 Uiso 1 1 calc GR . . . .
H30C H 0.0864 1.0271 0.8158 0.077 Uiso 1 1 calc GR . . . .
C31 C 0.6206(4) -0.3638(3) 0.5878(3) 0.0337(8) Uani 1 1 d . . . . .
C32 C 0.4096(3) -0.3055(3) 0.5840(3) 0.0270(7) Uani 1 1 d . . . . .
C33 C 0.6458(3) -0.1474(3) 0.6414(2) 0.0294(8) Uani 1 1 d . . . . .
P1 P 0.21230(10) 0.70104(8) 0.07950(7) 0.0348(2) Uani 1 1 d D . . . .
F1 F 0.2075(3) 0.6300(2) 0.1492(2) 0.0740(8) Uani 1 1 d D . . . .
F2 F 0.2178(3) 0.7740(2) 0.00977(18) 0.0649(7) Uani 1 1 d D . . . .
F3 F 0.3028(5) 0.6344(5) 0.0346(4) 0.0910(17) Uani 0.799(3) 1 d D . P A 1
F4 F 0.3180(5) 0.7989(4) 0.1680(3) 0.126(2) Uani 0.799(3) 1 d D . P A 1
F5 F 0.1135(4) 0.7634(4) 0.1169(3) 0.0769(13) Uani 0.799(3) 1 d D . P A 1
F6 F 0.0977(4) 0.6076(3) -0.0124(3) 0.0753(11) Uani 0.799(3) 1 d D . P A 1
F3A F 0.3607(19) 0.727(2) 0.0960(15) 0.0910(17) Uani 0.201(3) 1 d . . P A 2
F4A F 0.230(2) 0.8107(15) 0.1683(12) 0.126(2) Uani 0.201(3) 1 d D . P A 2
F5A F 0.0783(14) 0.6787(15) 0.0740(12) 0.0769(13) Uani 0.201(3) 1 d D . P A 2
F6A F 0.195(2) 0.5908(10) -0.0024(10) 0.0753(11) Uani 0.201(3) 1 d D . P A 2
O5 O 0.2983(3) 0.9257(2) 0.5219(2) 0.0573(8) Uani 1 1 d . . . . .
C34 C 0.2888(4) 0.8576(3) 0.4404(3) 0.0404(9) Uani 1 1 d . . . . .
C35 C 0.4026(4) 0.8441(3) 0.4083(3) 0.0490(10) Uani 1 1 d . . . . .
H35A H 0.4766 0.9042 0.4572 0.073 Uiso 1 1 calc GR . . . .
H35B H 0.3907 0.8506 0.3426 0.073 Uiso 1 1 calc GR . . . .
H35C H 0.4149 0.7686 0.4039 0.073 Uiso 1 1 calc GR . . . .
C36 C 0.1646(4) 0.7828(4) 0.3692(3) 0.0519(11) Uani 1 1 d . . . . .
H36A H 0.1609 0.7024 0.3598 0.078 Uiso 1 1 calc GR . . . .
H36B H 0.1535 0.7923 0.3047 0.078 Uiso 1 1 calc GR . . . .
H36C H 0.0976 0.8042 0.3961 0.078 Uiso 1 1 calc GR . . . .


_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 N5 2.351(3) . ?
Re1 C1 2.182(3) . ?
Re1 C4 2.126(3) . ?
Re1 C31 1.907(4) . ?
Re1 C32 1.958(4) . ?
Re1 C33 1.941(3) . ?
O1 C31 1.154(4) . ?
O2 C32 1.146(4) . ?
O3 C33 1.150(4) . ?
O4 C14 1.222(4) . ?
N1 C1 1.361(4) . ?
N1 C2 1.376(4) . ?
N1 C7 1.456(4) . ?
N2 C1 1.354(4) . ?
N2 C3 1.394(4) . ?
N2 C9 1.464(4) . ?
N3 C4 1.365(4) . ?
N3 C5 1.376(5) . ?
N3 C8 1.469(5) . ?
N4 C4 1.356(4) . ?
N4 C6 1.384(5) . ?
N4 C11 1.468(4) . ?
N5 C10 1.500(4) . ?
N5 C12 1.501(4) . ?
N5 C13 1.499(4) . ?
N6 C14 1.351(4) . ?
N6 C15 1.419(4) . ?
N7 C26 1.378(4) . ?
N7 C29 1.451(4) . ?
N7 C30 1.422(5) . ?
C2 C3 1.327(5) . ?
C5 C6 1.337(6) . ?
C7 C8 1.535(5) . ?
C9 C10 1.503(4) . ?
C11 C12 1.513(5) . ?
C13 C14 1.531(4) . ?
C15 C16 1.398(5) . ?
C15 C20 1.378(5) . ?
C16 C17 1.367(5) . ?
C17 C18 1.397(5) . ?
C18 C19 1.396(5) . ?
C18 C21 1.473(5) . ?
C19 C20 1.393(5) . ?
C21 C22 1.330(5) . ?
C22 C23 1.463(5) . ?
C23 C24 1.400(5) . ?
C23 C28 1.392(5) . ?
C24 C25 1.377(5) . ?
C25 C26 1.399(5) . ?
C26 C27 1.402(5) . ?
C27 C28 1.381(5) . ?
P1 F1 1.572(2) . ?
P1 F2 1.592(2) . ?
P1 F3 1.579(3) . ?
P1 F4 1.558(4) . ?
P1 F5 1.590(3) . ?
P1 F6 1.605(3) . ?
P1 F3A 1.603(19) . ?
P1 F4A 1.534(16) . ?
P1 F5A 1.476(13) . ?
P1 F6A 1.486(12) . ?
O5 C34 1.212(4) . ?
C34 C35 1.497(6) . ?
C34 C36 1.488(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
C1 Re1 N5 83.84(10) . . ?
C4 Re1 N5 88.50(11) . . ?
C4 Re1 C1 75.10(12) . . ?
C31 Re1 N5 174.80(11) . . ?
C31 Re1 C1 101.14(13) . . ?
C31 Re1 C4 94.23(14) . . ?
C31 Re1 C32 85.57(15) . . ?
C31 Re1 C33 83.43(14) . . ?
C32 Re1 N5 92.36(11) . . ?
C32 Re1 C1 97.00(12) . . ?
C32 Re1 C4 171.92(11) . . ?
C33 Re1 N5 91.90(11) . . ?
C33 Re1 C1 169.68(13) . . ?
C33 Re1 C4 95.44(13) . . ?
C33 Re1 C32 92.56(13) . . ?
C1 N1 C2 111.8(3) . . ?
C1 N1 C7 123.8(3) . . ?
C2 N1 C7 123.8(3) . . ?
C1 N2 C3 111.0(3) . . ?
C1 N2 C9 128.9(2) . . ?
C3 N2 C9 120.0(3) . . ?
C4 N3 C5 111.2(3) . . ?
C4 N3 C8 125.8(3) . . ?
C5 N3 C8 123.0(3) . . ?
C4 N4 C6 111.0(3) . . ?
C4 N4 C11 122.2(3) . . ?
C6 N4 C11 126.2(3) . . ?
C10 N5 Re1 108.55(18) . . ?
C10 N5 C12 110.7(2) . . ?
C12 N5 Re1 115.82(19) . . ?
C13 N5 Re1 104.98(17) . . ?
C13 N5 C10 106.9(2) . . ?
C13 N5 C12 109.4(2) . . ?
C14 N6 C15 129.9(3) . . ?
C26 N7 C29 119.8(3) . . ?
C26 N7 C30 120.2(3) . . ?
C30 N7 C29 117.8(3) . . ?
N1 C1 Re1 125.4(2) . . ?
N2 C1 Re1 129.0(2) . . ?
N2 C1 N1 103.4(3) . . ?
C3 C2 N1 106.8(3) . . ?
C2 C3 N2 107.0(3) . . ?
N3 C4 Re1 129.6(2) . . ?
N4 C4 Re1 125.0(2) . . ?
N4 C4 N3 103.8(3) . . ?
C6 C5 N3 106.9(3) . . ?
C5 C6 N4 107.0(3) . . ?
N1 C7 C8 113.8(3) . . ?
N3 C8 C7 115.8(3) . . ?
N2 C9 C10 116.2(3) . . ?
N5 C10 C9 116.7(3) . . ?
N4 C11 C12 111.6(3) . . ?
N5 C12 C11 114.2(3) . . ?
N5 C13 C14 119.1(2) . . ?
O4 C14 N6 124.9(3) . . ?
O4 C14 C13 125.6(3) . . ?
N6 C14 C13 109.5(3) . . ?
C16 C15 N6 115.8(3) . . ?
C20 C15 N6 125.1(3) . . ?
C20 C15 C16 119.0(3) . . ?
C17 C16 C15 121.1(3) . . ?
C16 C17 C18 121.1(3) . . ?
C17 C18 C21 122.2(3) . . ?
C19 C18 C17 117.3(3) . . ?
C19 C18 C21 120.4(3) . . ?
C20 C19 C18 121.9(3) . . ?
C15 C20 C19 119.6(3) . . ?
C22 C21 C18 125.5(3) . . ?
C21 C22 C23 128.0(3) . . ?
C24 C23 C22 119.0(3) . . ?
C28 C23 C22 124.3(3) . . ?
C28 C23 C24 116.6(3) . . ?
C25 C24 C23 122.1(3) . . ?
C24 C25 C26 121.3(3) . . ?
N7 C26 C25 121.6(3) . . ?
N7 C26 C27 121.8(3) . . ?
C25 C26 C27 116.6(3) . . ?
C28 C27 C26 121.6(3) . . ?
C27 C28 C23 121.7(3) . . ?
O1 C31 Re1 173.9(3) . . ?
O2 C32 Re1 174.3(3) . . ?
O3 C33 Re1 177.6(3) . . ?
F1 P1 F2 179.47(18) . . ?
F1 P1 F3 89.72(17) . . ?
F1 P1 F5 91.81(16) . . ?
F1 P1 F6 93.99(17) . . ?
F1 P1 F3A 96.9(6) . . ?
F2 P1 F6 86.52(16) . . ?
F2 P1 F3A 82.9(6) . . ?
F3 P1 F2 90.48(17) . . ?
F3 P1 F5 175.8(3) . . ?
F3 P1 F6 87.4(3) . . ?
F4 P1 F1 88.8(2) . . ?
F4 P1 F2 90.73(19) . . ?
F4 P1 F3 96.1(3) . . ?
F4 P1 F5 87.8(3) . . ?
F4 P1 F6 175.5(3) . . ?
F5 P1 F2 88.03(15) . . ?
F5 P1 F6 88.6(2) . . ?
F4A P1 F1 89.7(7) . . ?
F4A P1 F2 89.8(7) . . ?
F4A P1 F3A 92.1(11) . . ?
F5A P1 F1 78.9(5) . . ?
F5A P1 F2 101.3(5) . . ?
F5A P1 F3A 174.7(8) . . ?
F5A P1 F4A 84.8(10) . . ?
F5A P1 F6A 94.4(10) . . ?
F6A P1 F1 86.8(6) . . ?
F6A P1 F2 93.6(6) . . ?
F6A P1 F3A 88.4(10) . . ?
F6A P1 F4A 176.5(9) . . ?
O5 C34 C35 121.0(4) . . ?
O5 C34 C36 121.7(4) . . ?
C36 C34 C35 117.3(3) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
