# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_recofdu
_database_code_depnum_ccdc_archive 'CCDC 1457864'
_audit_update_record             
;
2016-07-07 deposited with the CCDC.
2016-08-16 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         'C19 H14 Cl2 N6 O8 Re2, 1.5(C7 H8)'
_chemical_formula_sum            'C29.50 H26 Cl2 N6 O8 Re2'
_chemical_formula_weight         1035.86

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'
Cl Cl 0.1484 0.1585 '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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-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                   32.2460(12)
_cell_length_b                   11.4564(13)
_cell_length_c                   21.046(2)
_cell_angle_alpha                90
_cell_angle_beta                 121.537(8)
_cell_angle_gamma                90
_cell_volume                     6626.5(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    206
_cell_measurement_theta_min      4
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_F_000             3944
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.1
-1 0 0 0.1
0 1 0 0.17
0 -1 0 0.17
3 2 0 0.09
-3 -2 0 0.09
-1 -1 8 0.1
1 1 -8 0.1
1 -1 0 0.134
-1 1 0 0.174

_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    7.520
_shelx_estimated_absorpt_T_min   0.162
_shelx_estimated_absorpt_T_max   0.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2.10, 2003)'
_exptl_absorpt_correction_T_min  0.1623
_exptl_absorpt_correction_T_max  0.3447
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            77899
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.261
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7603
_reflns_number_gt                6406
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0650P)²+25.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7603
_refine_ls_number_parameters     425
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.1234
_refine_ls_wR_factor_gt          0.1177
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_restrained_S_all      1.278
_refine_ls_shift/su_max          0.004
_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 0.34762(2) 0.57708(2) 0.57703(2) 0.02610(10) Uani 1 1 d . . . . .
Cl1 Cl 0.33210(8) 0.60950(15) 0.44889(10) 0.0362(4) Uani 1 1 d . . . . .
C7X C 0.3605(3) 0.5469(7) 0.6745(5) 0.0360(18) Uani 1 1 d . . . . .
O7X O 0.3678(2) 0.5272(6) 0.7338(4) 0.0504(16) Uani 1 1 d . . . . .
C8X C 0.3127(3) 0.7147(7) 0.5752(4) 0.0352(17) Uani 1 1 d . . . . .
O8X O 0.2931(2) 0.7981(5) 0.5758(4) 0.0487(16) Uani 1 1 d . . . . .
C9X C 0.2881(3) 0.4877(7) 0.5365(5) 0.0341(17) Uani 1 1 d . . . . .
O9X O 0.2536(2) 0.4322(5) 0.5103(4) 0.0488(16) Uani 1 1 d . . . . .
Re2 Re 0.40017(2) 0.17919(2) 0.63685(2) 0.02263(9) Uani 1 1 d . . . . .
Cl2 Cl 0.46539(7) 0.14422(16) 0.61080(11) 0.0337(4) Uani 1 1 d . . . . .
C7Y C 0.3442(3) 0.2043(6) 0.6456(4) 0.0290(16) Uani 1 1 d . . . . .
O7Y O 0.3130(2) 0.2235(6) 0.6534(4) 0.0468(15) Uani 1 1 d . . . . .
C8Y C 0.4202(3) 0.0434(7) 0.7023(4) 0.0319(16) Uani 1 1 d . . . . .
O8Y O 0.4331(2) -0.0325(5) 0.7415(3) 0.0363(13) Uani 1 1 d . . . . .
C9Y C 0.4368(3) 0.2764(6) 0.7211(4) 0.0287(15) Uani 1 1 d . . . . .
O9Y O 0.4566(2) 0.3424(5) 0.7704(3) 0.0385(13) Uani 1 1 d . . . . .
N1 N 0.2622(2) 0.1541(5) 0.3196(3) 0.0280(13) Uani 1 1 d . . . . .
C1 C 0.2244(3) 0.1740(7) 0.2411(4) 0.0385(19) Uani 1 1 d . . . . .
H1A H 0.2110 0.1004 0.2173 0.058 Uiso 1 1 d R U . . .
H1B H 0.1991 0.2217 0.2385 0.058 Uiso 1 1 d R U . . .
H1C H 0.2384 0.2127 0.2162 0.058 Uiso 1 1 d R U . . .
C2 C 0.2721(3) 0.0386(6) 0.3439(4) 0.0264(14) Uani 1 1 d . . . . .
O2 O 0.2510(2) -0.0425(5) 0.3014(3) 0.0365(13) Uani 1 1 d . . . . .
N3 N 0.3055(2) 0.0191(5) 0.4176(3) 0.0268(13) Uani 1 1 d . . . . .
C3 C 0.3159(3) -0.1038(6) 0.4422(5) 0.042(2) Uani 1 1 d . . . . .
H3A H 0.3398 -0.1063 0.4946 0.064 Uiso 1 1 d R U . . .
H3B H 0.2865 -0.1409 0.4330 0.064 Uiso 1 1 d R U . . .
H3C H 0.3281 -0.1439 0.4153 0.064 Uiso 1 1 d R U . . .
C4 C 0.3293(3) 0.1069(6) 0.4697(4) 0.0244(14) Uani 1 1 d . . . . .
O4 O 0.35795(18) 0.0766(4) 0.5354(3) 0.0265(11) Uani 1 1 d . . . . .
C5 C 0.3202(2) 0.2237(6) 0.4419(4) 0.0228(13) Uani 1 1 d . . . . .
C6 C 0.2869(3) 0.2448(6) 0.3662(4) 0.0259(14) Uani 1 1 d . . . . .
N6 N 0.2769(2) 0.3505(5) 0.3354(4) 0.0349(15) Uani 1 1 d . . . . .
H6A H 0.2557 0.3587 0.2887 0.042 Uiso 1 1 d R U . . .
H6B H 0.2916 0.4107 0.3623 0.042 Uiso 1 1 d R U . . .
C51 C 0.3466(3) 0.3208(6) 0.4871(4) 0.0265(15) Uani 1 1 d . . . . .
H51 H 0.3407 0.3922 0.4628 0.032 Uiso 1 1 d R U . . .
N51 N 0.3780(2) 0.3212(4) 0.5582(3) 0.0227(12) Uani 1 1 d . . . . .
N52 N 0.3948(2) 0.4368(5) 0.5833(3) 0.0224(12) Uani 1 1 d . . . . .
C52 C 0.4400(3) 0.4571(6) 0.6125(4) 0.0244(14) Uani 1 1 d . . . . .
H52 H 0.4621 0.3978 0.6215 0.029 Uiso 1 1 d R U . . .
N1F N 0.4187(2) 0.6555(5) 0.6168(3) 0.0282(13) Uani 1 1 d . . . . .
C2F C 0.4555(3) 0.5791(6) 0.6314(4) 0.0273(15) Uani 1 1 d . . . . .
C3F C 0.5020(3) 0.6149(7) 0.6569(4) 0.0314(16) Uani 1 1 d . . . . .
H3F H 0.5262 0.5612 0.6666 0.038 Uiso 1 1 d R U . . .
C4F C 0.5124(3) 0.7343(7) 0.6677(4) 0.0347(17) Uani 1 1 d . . . . .
H4F H 0.5441 0.7605 0.6868 0.042 Uiso 1 1 d R U . . .
C5F C 0.4754(3) 0.8137(7) 0.6501(4) 0.0366(18) Uani 1 1 d . . . . .
H5F H 0.4812 0.8937 0.6545 0.044 Uiso 1 1 d R U . . .
C6F C 0.4294(3) 0.7690(7) 0.6260(4) 0.0319(16) Uani 1 1 d . . . . .
H6F H 0.4046 0.8213 0.6157 0.038 Uiso 1 1 d R U . . .
C1S C 0.1018(4) 0.5155(10) 0.1226(7) 0.062(3) Uani 1 1 d . . . . .
C2S C 0.1360(5) 0.4749(11) 0.1920(8) 0.071(4) Uani 1 1 d . . . . .
H2S H 0.1400 0.3949 0.2006 0.085 Uiso 1 1 d R U . . .
C3S C 0.1655(4) 0.5536(13) 0.2516(7) 0.073(4) Uani 1 1 d . . . . .
H3S H 0.1887 0.5252 0.2984 0.088 Uiso 1 1 d R U . . .
C4S C 0.1593(4) 0.6685(13) 0.2393(7) 0.070(3) Uani 1 1 d . . . . .
H4S H 0.1780 0.7201 0.2781 0.084 Uiso 1 1 d R U . . .
C5S C 0.1261(4) 0.7108(11) 0.1701(6) 0.059(3) Uani 1 1 d . . . . .
H5S H 0.1229 0.7911 0.1623 0.071 Uiso 1 1 d R U . . .
C6S C 0.0966(4) 0.6346(11) 0.1107(7) 0.062(3) Uani 1 1 d . . . . .
H6S H 0.0738 0.6642 0.0640 0.075 Uiso 1 1 d R U . . .
C7S C 0.0683(5) 0.4308(12) 0.0600(8) 0.081(4) Uani 1 1 d . . . . .
H7S1 H 0.0468 0.4742 0.0157 0.097 Uiso 1 1 d R U . . .
H7S2 H 0.0877 0.3787 0.0501 0.097 Uiso 1 1 d R U . . .
H7S3 H 0.0496 0.3864 0.0749 0.097 Uiso 1 1 d R U . . .
C1T C 0.5327(6) 0.4449(15) 0.5421(11) 0.046(5) Uiso 0.5 1 d D . P A -1
C2T C 0.4860(7) 0.397(2) 0.5097(12) 0.053(5) Uiso 0.5 1 d D . P A -1
H2T H 0.4823 0.3215 0.5218 0.064 Uiso 0.5 1 d R U P A -1
C3T C 0.4451(9) 0.4621(18) 0.4589(13) 0.060(6) Uiso 0.5 1 d D . P A -1
H3T H 0.4142 0.4301 0.4383 0.071 Uiso 0.5 1 d R U P A -1
C4T C 0.4486(8) 0.5752(19) 0.4380(15) 0.070(7) Uiso 0.5 1 d D . P A -1
H4T H 0.4213 0.6179 0.4043 0.084 Uiso 0.5 1 d R U P A -1
C5T C 0.4951(7) 0.6209(17) 0.4689(11) 0.046(5) Uiso 0.5 1 d D . P A -1
H5T H 0.4987 0.6950 0.4544 0.055 Uiso 0.5 1 d R U P A -1
C6T C 0.5364(8) 0.5593(15) 0.5217(11) 0.047(5) Uiso 0.5 1 d D . P A -1
H6T H 0.5671 0.5935 0.5445 0.056 Uiso 0.5 1 d R U P A -1
C7T C 0.5790(12) 0.381(3) 0.601(2) 0.105(10) Uiso 0.5 1 d . . P A -1
H71T H 0.6069 0.4298 0.6153 0.125 Uiso 0.5 1 d R U P A -1
H72T H 0.5823 0.3098 0.5798 0.125 Uiso 0.5 1 d R U P A -1
H73T H 0.5767 0.3642 0.6432 0.125 Uiso 0.5 1 d R U P A -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 C7X 1.900(9) . ?
Re1 C8X 1.926(8) . ?
Re1 C9X 1.935(8) . ?
Re1 N52 2.170(6) . ?
Re1 N1F 2.180(6) . ?
Re1 Cl1 2.500(2) . ?
C7X O7X 1.165(10) . ?
C8X O8X 1.149(9) . ?
C9X O9X 1.143(10) . ?
Re2 C9Y 1.895(8) . ?
Re2 C7Y 1.930(8) . ?
Re2 C8Y 1.950(8) . ?
Re2 N51 2.159(5) . ?
Re2 O4 2.180(5) . ?
Re2 Cl2 2.468(2) . ?
C7Y O7Y 1.120(9) . ?
C8Y O8Y 1.119(9) . ?
C9Y O9Y 1.167(9) . ?
N1 C6 1.364(9) . ?
N1 C2 1.394(9) . ?
N1 C1 1.470(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O2 1.222(8) . ?
C2 N3 1.366(9) . ?
N3 C4 1.387(9) . ?
N3 C3 1.477(9) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 O4 1.245(8) . ?
C4 C5 1.428(9) . ?
C5 C6 1.401(10) . ?
C5 C51 1.421(9) . ?
C6 N6 1.331(9) . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
C51 N51 1.296(9) . ?
C51 H51 0.9300 . ?
N51 N52 1.423(7) . ?
N52 C52 1.272(9) . ?
C52 C2F 1.467(9) . ?
C52 H52 0.9300 . ?
N1F C6F 1.333(9) . ?
N1F C2F 1.374(9) . ?
C2F C3F 1.365(10) . ?
C3F C4F 1.398(10) . ?
C3F H3F 0.9300 . ?
C4F C5F 1.388(12) . ?
C4F H4F 0.9300 . ?
C5F C6F 1.391(11) . ?
C5F H5F 0.9300 . ?
C6F H6F 0.9300 . ?
C1S C2S 1.371(16) . ?
C1S C6S 1.382(16) . ?
C1S C7S 1.536(17) . ?
C2S C3S 1.429(19) . ?
C2S H2S 0.9300 . ?
C3S C4S 1.336(18) . ?
C3S H3S 0.9300 . ?
C4S C5S 1.368(16) . ?
C4S H4S 0.9300 . ?
C5S C6S 1.408(17) . ?
C5S H5S 0.9300 . ?
C6S H6S 0.9300 . ?
C7S H7S1 0.9600 . ?
C7S H7S2 0.9600 . ?
C7S H7S3 0.9600 . ?
C1T C2T 1.399(10) . ?
C1T C6T 1.404(10) . ?
C1T C7T 1.53(4) . ?
C2T C3T 1.399(10) . ?
C2T H2T 0.9300 . ?
C3T C4T 1.391(10) . ?
C3T H3T 0.9301 . ?
C4T C5T 1.388(10) . ?
C4T H4T 0.9300 . ?
C5T C6T 1.400(10) . ?
C5T H5T 0.9300 . ?
C6T H6T 0.9300 . ?
C7T H71T 0.9600 . ?
C7T H72T 0.9600 . ?
C7T H73T 0.9600 . ?

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
C7X Re1 C8X 88.1(3) . . ?
C7X Re1 C9X 89.2(4) . . ?
C8X Re1 C9X 89.4(3) . . ?
C7X Re1 N52 92.8(3) . . ?
C8X Re1 N52 172.7(3) . . ?
C9X Re1 N52 97.9(3) . . ?
C7X Re1 N1F 93.9(3) . . ?
C8X Re1 N1F 99.0(3) . . ?
C9X Re1 N1F 171.1(3) . . ?
N52 Re1 N1F 73.7(2) . . ?
C7X Re1 Cl1 177.8(2) . . ?
C8X Re1 Cl1 94.1(2) . . ?
C9X Re1 Cl1 90.6(3) . . ?
N52 Re1 Cl1 85.06(15) . . ?
N1F Re1 Cl1 85.98(17) . . ?
O7X C7X Re1 179.1(8) . . ?
O8X C8X Re1 177.9(8) . . ?
O9X C9X Re1 176.6(7) . . ?
C9Y Re2 C7Y 88.8(3) . . ?
C9Y Re2 C8Y 89.7(3) . . ?
C7Y Re2 C8Y 91.9(3) . . ?
C9Y Re2 N51 94.0(3) . . ?
C7Y Re2 N51 90.6(3) . . ?
C8Y Re2 N51 175.7(3) . . ?
C9Y Re2 O4 176.3(2) . . ?
C7Y Re2 O4 92.1(3) . . ?
C8Y Re2 O4 93.9(3) . . ?
N51 Re2 O4 82.46(19) . . ?
C9Y Re2 Cl2 96.7(2) . . ?
C7Y Re2 Cl2 173.7(2) . . ?
C8Y Re2 Cl2 91.2(2) . . ?
N51 Re2 Cl2 86.01(17) . . ?
O4 Re2 Cl2 82.14(14) . . ?
O7Y C7Y Re2 176.2(7) . . ?
O8Y C8Y Re2 177.6(8) . . ?
O9Y C9Y Re2 175.0(7) . . ?
C6 N1 C2 121.6(6) . . ?
C6 N1 C1 121.3(6) . . ?
C2 N1 C1 117.1(6) . . ?
N1 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.6 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 N3 120.9(7) . . ?
O2 C2 N1 121.3(7) . . ?
N3 C2 N1 117.8(6) . . ?
C2 N3 C4 124.1(6) . . ?
C2 N3 C3 117.0(6) . . ?
C4 N3 C3 118.9(6) . . ?
N3 C3 H3A 109.3 . . ?
N3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N3 C3 H3C 109.6 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 N3 117.3(6) . . ?
O4 C4 C5 126.2(6) . . ?
N3 C4 C5 116.5(6) . . ?
C4 O4 Re2 131.2(4) . . ?
C6 C5 C51 117.4(6) . . ?
C6 C5 C4 119.9(6) . . ?
C51 C5 C4 122.4(6) . . ?
N6 C6 N1 116.2(6) . . ?
N6 C6 C5 123.9(6) . . ?
N1 C6 C5 119.9(6) . . ?
C6 N6 H6A 120.1 . . ?
C6 N6 H6B 119.9 . . ?
H6A N6 H6B 120.0 . . ?
N51 C51 C5 127.5(6) . . ?
N51 C51 H51 116.3 . . ?
C5 C51 H51 116.2 . . ?
C51 N51 N52 110.4(5) . . ?
C51 N51 Re2 128.9(5) . . ?
N52 N51 Re2 120.5(4) . . ?
C52 N52 N51 117.9(6) . . ?
C52 N52 Re1 118.9(4) . . ?
N51 N52 Re1 123.2(4) . . ?
N52 C52 C2F 116.5(6) . . ?
N52 C52 H52 121.8 . . ?
C2F C52 H52 121.7 . . ?
C6F N1F C2F 117.4(6) . . ?
C6F N1F Re1 126.7(5) . . ?
C2F N1F Re1 115.8(5) . . ?
C3F C2F N1F 122.7(7) . . ?
C3F C2F C52 122.7(7) . . ?
N1F C2F C52 114.5(6) . . ?
C2F C3F C4F 118.6(7) . . ?
C2F C3F H3F 120.8 . . ?
C4F C3F H3F 120.7 . . ?
C5F C4F C3F 119.9(7) . . ?
C5F C4F H4F 120.0 . . ?
C3F C4F H4F 120.1 . . ?
C4F C5F C6F 117.4(7) . . ?
C4F C5F H5F 121.3 . . ?
C6F C5F H5F 121.4 . . ?
N1F C6F C5F 124.0(7) . . ?
N1F C6F H6F 118.0 . . ?
C5F C6F H6F 118.1 . . ?
C2S C1S C6S 118.8(12) . . ?
C2S C1S C7S 120.8(12) . . ?
C6S C1S C7S 120.3(11) . . ?
C1S C2S C3S 121.1(11) . . ?
C1S C2S H2S 119.6 . . ?
C3S C2S H2S 119.4 . . ?
C4S C3S C2S 119.2(12) . . ?
C4S C3S H3S 120.5 . . ?
C2S C3S H3S 120.4 . . ?
C3S C4S C5S 120.7(14) . . ?
C3S C4S H4S 119.5 . . ?
C5S C4S H4S 119.8 . . ?
C4S C5S C6S 120.9(12) . . ?
C4S C5S H5S 119.3 . . ?
C6S C5S H5S 119.8 . . ?
C1S C6S C5S 119.3(11) . . ?
C1S C6S H6S 120.4 . . ?
C5S C6S H6S 120.3 . . ?
C1S C7S H7S1 109.4 . . ?
C1S C7S H7S2 109.5 . . ?
H7S1 C7S H7S2 109.5 . . ?
C1S C7S H7S3 109.5 . . ?
H7S1 C7S H7S3 109.5 . . ?
H7S2 C7S H7S3 109.5 . . ?
C2T C1T C6T 117.2(17) . . ?
C2T C1T C7T 124(2) . . ?
C6T C1T C7T 119(2) . . ?
C3T C2T C1T 121(2) . . ?
C3T C2T H2T 120.0 . . ?
C1T C2T H2T 119.3 . . ?
C4T C3T C2T 122(2) . . ?
C4T C3T H3T 117.6 . . ?
C2T C3T H3T 119.9 . . ?
C5T C4T C3T 117(2) . . ?
C5T C4T H4T 121.3 . . ?
C3T C4T H4T 122.0 . . ?
C4T C5T C6T 122(2) . . ?
C4T C5T H5T 118.7 . . ?
C6T C5T H5T 119.4 . . ?
C5T C6T C1T 121.0(18) . . ?
C5T C6T H6T 120.7 . . ?
C1T C6T H6T 118.3 . . ?
C1T C7T H71T 109.7 . . ?
C1T C7T H72T 109.5 . . ?
H71T C7T H72T 109.5 . . ?
C1T C7T H73T 109.2 . . ?
H71T C7T H73T 109.5 . . ?
H72T C7T H73T 109.5 . . ?

_refine_diff_density_max         2.386
_refine_diff_density_min         -2.176
_refine_diff_density_rms         0.312

# start Validation Reply Form
_vrf_PLAT414_recofdu             
;
PROBLEM: Short Intra D-H..H-X       H6B    ..  H51     ..       1.88 Ang.  
RESPONSE: The close position of these two atoms is forced by the geometry of
  the molecule.
;
_vrf_PLAT910_recofdu             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          12 Note  
RESPONSE: The effective value of theta(min) has been increased to remove
   reflections that were absorbed by the beamstop.
;
_vrf_PLAT934_recofdu             
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....         10 Check 
RESPONSE: We do not think that the number of these "bad" reflections is
          too high.
;
# end Validation Reply Form


####################################################################### 
# 
# 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_refdudmso
_database_code_depnum_ccdc_archive 'CCDC 1457865'
_audit_update_record             
;
2016-07-07 deposited with the CCDC.
2016-08-16 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         'C19 H15 Cl N6 O9 Re2, 2(C2 H6 O S)'
_chemical_formula_sum            'C23 H27 Cl N6 O11 Re2 S2'
_chemical_formula_weight         1035.47

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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.0852(17)
_cell_length_b                   20.8164(5)
_cell_length_c                   13.6738(15)
_cell_angle_alpha                90
_cell_angle_beta                 112.846(9)
_cell_angle_gamma                90
_cell_volume                     3170.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    135
_cell_measurement_theta_min      4
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.170
_exptl_crystal_F_000             1976
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.07
-1 0 0 0.05
0 1 0 0.07
0 -1 0 0.09
0 0 1 0.08
0 0 -1 0.08
0 -2 -1 0.087
0 3 -1 0.039

_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    7.911
_shelx_estimated_absorpt_T_min   0.263
_shelx_estimated_absorpt_T_max   0.404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_absorpt_correction_T_min  0.2634
_exptl_absorpt_correction_T_max  0.4039
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46847
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.538
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7273
_reflns_number_gt                4496
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0500P)²+20.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7273
_refine_ls_number_parameters     412
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1281
_refine_ls_wR_factor_gt          0.1052
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_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 0.29799(3) 0.56130(2) 0.17030(3) 0.01923(11) Uani 1 1 d . . . . .
Cl1 Cl 0.2118(2) 0.66637(12) 0.1909(2) 0.0306(6) Uani 1 1 d . . . . .
C7X C 0.3663(8) 0.4841(4) 0.1433(7) 0.0199(19) Uani 1 1 d . . . . .
O7X O 0.4085(6) 0.4364(3) 0.1301(5) 0.0286(15) Uani 1 1 d . . . . .
C8X C 0.1468(9) 0.5191(4) 0.1323(8) 0.030(2) Uani 1 1 d . . . . .
O8X O 0.0546(6) 0.4947(3) 0.1142(6) 0.0351(17) Uani 1 1 d . . . . .
C9X C 0.3363(8) 0.5300(4) 0.3127(8) 0.025(2) Uani 1 1 d . . . . .
O9X O 0.3617(6) 0.5083(3) 0.3947(5) 0.0292(15) Uani 1 1 d . . . . .
Re2 Re 0.71737(3) 0.55796(2) 0.33386(3) 0.01873(11) Uani 1 1 d . . . . .
C7Y C 0.6445(8) 0.4801(5) 0.3529(7) 0.024(2) Uani 1 1 d . . . . .
O7Y O 0.5992(6) 0.4331(3) 0.3629(5) 0.0324(16) Uani 1 1 d . . . . .
C8Y C 0.8646(8) 0.5126(4) 0.3615(7) 0.023(2) Uani 1 1 d . . . . .
O8Y O 0.9531(6) 0.4856(3) 0.3748(6) 0.0349(17) Uani 1 1 d . . . . .
C9Y C 0.6673(8) 0.5353(4) 0.1866(8) 0.024(2) Uani 1 1 d . . . . .
O9Y O 0.6342(6) 0.5199(3) 0.0982(5) 0.0303(16) Uani 1 1 d . . . . .
O1W O 0.7960(6) 0.6526(3) 0.3245(5) 0.0256(15) Uani 1 1 d D . . . .
H11W H 0.777(9) 0.675(4) 0.268(4) 0.031 Uiso 1 1 d D U . . .
H12W H 0.860(5) 0.659(5) 0.379(4) 0.031 Uiso 1 1 d D U . . .
N1 N 0.7756(6) 0.6343(4) 0.6513(6) 0.0210(17) Uani 1 1 d . . . . .
C1 C 0.9032(8) 0.6202(5) 0.7050(7) 0.033(2) Uani 1 1 d . . . . .
H04A H 0.9302 0.6325 0.7799 0.049 Uiso 1 1 d R U . . .
H04B H 0.9167 0.5742 0.6997 0.049 Uiso 1 1 d R U . . .
H04C H 0.9484 0.6446 0.6715 0.049 Uiso 1 1 d R U . . .
C2 C 0.7193(8) 0.6595(4) 0.7139(8) 0.026(2) Uani 1 1 d . . . . .
O2 O 0.7734(6) 0.6671(3) 0.8103(5) 0.0326(16) Uani 1 1 d . . . . .
N3 N 0.6003(7) 0.6779(3) 0.6648(6) 0.0221(17) Uani 1 1 d . . . . .
C3 C 0.5443(8) 0.7052(5) 0.7325(8) 0.027(2) Uani 1 1 d . . . . .
H03A H 0.4607 0.7164 0.6892 0.041 Uiso 1 1 d R U . . .
H03B H 0.5465 0.6736 0.7864 0.041 Uiso 1 1 d R U . . .
H03C H 0.5881 0.7439 0.7674 0.041 Uiso 1 1 d R U . . .
C4 C 0.5351(8) 0.6750(4) 0.5547(7) 0.023(2) Uani 1 1 d . . . . .
O4 O 0.4325(6) 0.6967(3) 0.5162(5) 0.0294(16) Uani 1 1 d . . . . .
C5 C 0.5945(7) 0.6443(4) 0.4924(7) 0.0192(19) Uani 1 1 d . . . . .
C6 C 0.7151(8) 0.6214(4) 0.5442(8) 0.024(2) Uani 1 1 d . . . . .
N6 N 0.7714(7) 0.5889(4) 0.4944(6) 0.0240(18) Uani 1 1 d . . . . .
H6 H 0.8453 0.5779 0.5353 0.029 Uiso 1 1 d R U . . .
C51 C 0.5262(8) 0.6392(4) 0.3833(7) 0.0203(19) Uani 1 1 d . . . . .
H51 H 0.4468 0.6557 0.3594 0.024 Uiso 1 1 d R U . . .
N51 N 0.5587(6) 0.6143(3) 0.3092(6) 0.0197(16) Uani 1 1 d . . . . .
N52 N 0.4642(6) 0.6136(3) 0.2084(6) 0.0177(16) Uani 1 1 d . . . . .
C52 C 0.4856(8) 0.6405(4) 0.1313(7) 0.0184(19) Uani 1 1 d . . . . .
H52 H 0.5592 0.6620 0.1439 0.022 Uiso 1 1 d R U . . .
N1F N 0.2916(6) 0.6018(3) 0.0197(6) 0.0193(16) Uani 1 1 d . . . . .
C2F C 0.3915(8) 0.6360(4) 0.0248(7) 0.021(2) Uani 1 1 d . . . . .
C3F C 0.4049(8) 0.6609(5) -0.0615(7) 0.026(2) Uani 1 1 d . . . . .
H3F H 0.4759 0.6838 -0.0537 0.031 Uiso 1 1 d R U . . .
C4F C 0.3144(8) 0.6528(5) -0.1615(8) 0.030(2) Uani 1 1 d . . . . .
H4F H 0.3222 0.6690 -0.2234 0.036 Uiso 1 1 d R U . . .
C5F C 0.2124(8) 0.6203(4) -0.1670(7) 0.024(2) Uani 1 1 d . . . . .
H5F H 0.1473 0.6154 -0.2336 0.029 Uiso 1 1 d R U . . .
C6F C 0.2040(8) 0.5948(4) -0.0770(7) 0.022(2) Uani 1 1 d . . . . .
H6F H 0.1338 0.5716 -0.0836 0.027 Uiso 1 1 d R U . . .
S1S S 0.7615(2) 0.67965(12) 0.0330(2) 0.0269(5) Uani 1 1 d . . . . .
O1S O 0.7410(6) 0.6950(3) 0.1337(6) 0.0328(17) Uani 1 1 d . . . . .
C11S C 0.8562(9) 0.6105(5) 0.0613(9) 0.037(3) Uani 1 1 d . . . . .
H11A H 0.8717 0.5989 -0.0017 0.055 Uiso 1 1 d R U . . .
H11B H 0.9324 0.6200 0.1202 0.055 Uiso 1 1 d R U . . .
H11C H 0.8165 0.5745 0.0808 0.055 Uiso 1 1 d R U . . .
C12S C 0.8704(8) 0.7356(5) 0.0294(9) 0.035(3) Uani 1 1 d . . . . .
H12A H 0.8874 0.7281 -0.0341 0.052 Uiso 1 1 d R U . . .
H12B H 0.8397 0.7793 0.0275 0.052 Uiso 1 1 d R U . . .
H12C H 0.9443 0.7303 0.0928 0.052 Uiso 1 1 d R U . . .
S2S S 1.1372(2) 0.66112(12) 0.5118(2) 0.0282(6) Uani 1 1 d . . . . .
O2S O 1.0054(5) 0.6505(3) 0.4918(5) 0.0331(17) Uani 1 1 d . . . . .
C21S C 1.1455(9) 0.7337(5) 0.4493(9) 0.039(3) Uani 1 1 d . . . . .
H21A H 1.2292 0.7424 0.4604 0.059 Uiso 1 1 d R U . . .
H21B H 1.0969 0.7305 0.3731 0.059 Uiso 1 1 d R U . . .
H21C H 1.1150 0.7688 0.4797 0.059 Uiso 1 1 d R U . . .
C22S C 1.1710(9) 0.6076(5) 0.4277(8) 0.033(2) Uani 1 1 d . . . . .
H22A H 1.2554 0.6127 0.4378 0.050 Uiso 1 1 d R U . . .
H22B H 1.1571 0.5634 0.4449 0.050 Uiso 1 1 d R U . . .
H22C H 1.1194 0.6170 0.3537 0.050 Uiso 1 1 d R U . . .


_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 C7X 1.906(9) . ?
Re1 C8X 1.908(10) . ?
Re1 C9X 1.931(10) . ?
Re1 N52 2.162(7) . ?
Re1 N1F 2.199(7) . ?
Re1 Cl1 2.485(2) . ?
C7X O7X 1.162(10) . ?
C8X O8X 1.161(11) . ?
C9X O9X 1.135(11) . ?
Re2 C7Y 1.911(10) . ?
Re2 C8Y 1.918(9) . ?
Re2 C9Y 1.923(10) . ?
Re2 N6 2.133(7) . ?
Re2 N51 2.160(7) . ?
Re2 O1W 2.212(7) . ?
C7Y O7Y 1.154(10) . ?
C8Y O8Y 1.159(10) . ?
C9Y O9Y 1.162(10) . ?
O1W H11W 0.848(10) . ?
O1W H12W 0.850(10) . ?
N1 C6 1.386(11) . ?
N1 C2 1.388(11) . ?
N1 C1 1.457(11) . ?
C1 H04A 0.9800 . ?
C1 H04B 0.9800 . ?
C1 H04C 0.9800 . ?
C2 O2 1.233(11) . ?
C2 N3 1.384(11) . ?
N3 C4 1.404(11) . ?
N3 C3 1.457(11) . ?
C3 H03A 0.9800 . ?
C3 H03B 0.9800 . ?
C3 H03C 0.9800 . ?
C4 O4 1.230(11) . ?
C4 C5 1.459(12) . ?
C5 C51 1.400(12) . ?
C5 C6 1.432(12) . ?
C6 N6 1.320(11) . ?
N6 H6 0.8800 . ?
C51 N51 1.326(11) . ?
C51 H51 0.9500 . ?
N51 N52 1.408(10) . ?
N52 C52 1.305(10) . ?
C52 C2F 1.462(12) . ?
C52 H52 0.9500 . ?
N1F C6F 1.342(11) . ?
N1F C2F 1.381(11) . ?
C2F C3F 1.354(12) . ?
C3F C4F 1.391(13) . ?
C3F H3F 0.9500 . ?
C4F C5F 1.382(12) . ?
C4F H4F 0.9500 . ?
C5F C6F 1.380(12) . ?
C5F H5F 0.9500 . ?
C6F H6F 0.9500 . ?
S1S O1S 1.524(7) . ?
S1S C12S 1.773(9) . ?
S1S C11S 1.786(10) . ?
C11S H11A 0.9800 . ?
C11S H11B 0.9800 . ?
C11S H11C 0.9800 . ?
C12S H12A 0.9800 . ?
C12S H12B 0.9800 . ?
C12S H12C 0.9800 . ?
S2S O2S 1.523(6) . ?
S2S C21S 1.758(10) . ?
S2S C22S 1.758(10) . ?
C21S H21A 0.9800 . ?
C21S H21B 0.9800 . ?
C21S H21C 0.9800 . ?
C22S H22A 0.9800 . ?
C22S H22B 0.9800 . ?
C22S H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7X Re1 C8X 90.0(4) . . ?
C7X Re1 C9X 87.6(4) . . ?
C8X Re1 C9X 87.0(4) . . ?
C7X Re1 N52 92.2(3) . . ?
C8X Re1 N52 176.9(3) . . ?
C9X Re1 N52 95.2(3) . . ?
C7X Re1 N1F 90.1(3) . . ?
C8X Re1 N1F 103.8(3) . . ?
C9X Re1 N1F 168.9(3) . . ?
N52 Re1 N1F 74.0(3) . . ?
C7X Re1 Cl1 174.6(3) . . ?
C8X Re1 Cl1 92.1(3) . . ?
C9X Re1 Cl1 97.5(3) . . ?
N52 Re1 Cl1 85.47(18) . . ?
N1F Re1 Cl1 84.55(18) . . ?
O7X C7X Re1 177.8(8) . . ?
O8X C8X Re1 176.2(9) . . ?
O9X C9X Re1 175.8(8) . . ?
C7Y Re2 C8Y 89.8(4) . . ?
C7Y Re2 C9Y 87.7(4) . . ?
C8Y Re2 C9Y 88.6(4) . . ?
C7Y Re2 N6 95.1(3) . . ?
C8Y Re2 N6 93.2(3) . . ?
C9Y Re2 N6 176.6(3) . . ?
C7Y Re2 N51 93.1(3) . . ?
C8Y Re2 N51 176.2(3) . . ?
C9Y Re2 N51 94.1(3) . . ?
N6 Re2 N51 84.0(3) . . ?
C7Y Re2 O1W 174.0(3) . . ?
C8Y Re2 O1W 93.7(3) . . ?
C9Y Re2 O1W 97.2(3) . . ?
N6 Re2 O1W 79.9(3) . . ?
N51 Re2 O1W 83.3(2) . . ?
O7Y C7Y Re2 179.0(9) . . ?
O8Y C8Y Re2 177.7(8) . . ?
O9Y C9Y Re2 177.4(8) . . ?
Re2 O1W H11W 125(7) . . ?
Re2 O1W H12W 110(7) . . ?
H11W O1W H12W 123(10) . . ?
C6 N1 C2 122.8(7) . . ?
C6 N1 C1 121.0(7) . . ?
C2 N1 C1 116.2(7) . . ?
N1 C1 H04A 109.5 . . ?
N1 C1 H04B 109.5 . . ?
H04A C1 H04B 109.5 . . ?
N1 C1 H04C 109.5 . . ?
H04A C1 H04C 109.5 . . ?
H04B C1 H04C 109.5 . . ?
O2 C2 N3 120.2(9) . . ?
O2 C2 N1 121.6(8) . . ?
N3 C2 N1 118.1(8) . . ?
C2 N3 C4 123.6(8) . . ?
C2 N3 C3 116.8(8) . . ?
C4 N3 C3 119.5(7) . . ?
N3 C3 H03A 109.5 . . ?
N3 C3 H03B 109.5 . . ?
H03A C3 H03B 109.5 . . ?
N3 C3 H03C 109.5 . . ?
H03A C3 H03C 109.5 . . ?
H03B C3 H03C 109.5 . . ?
O4 C4 N3 119.7(8) . . ?
O4 C4 C5 123.7(8) . . ?
N3 C4 C5 116.6(8) . . ?
C51 C5 C6 124.6(8) . . ?
C51 C5 C4 115.8(8) . . ?
C6 C5 C4 119.6(8) . . ?
N6 C6 N1 118.6(8) . . ?
N6 C6 C5 123.0(9) . . ?
N1 C6 C5 118.4(8) . . ?
C6 N6 Re2 132.2(7) . . ?
C6 N6 H6 113.9 . . ?
Re2 N6 H6 113.9 . . ?
N51 C51 C5 128.0(8) . . ?
N51 C51 H51 116.0 . . ?
C5 C51 H51 116.0 . . ?
C51 N51 N52 112.6(7) . . ?
C51 N51 Re2 127.0(6) . . ?
N52 N51 Re2 118.7(5) . . ?
C52 N52 N51 116.5(7) . . ?
C52 N52 Re1 118.6(6) . . ?
N51 N52 Re1 124.4(5) . . ?
N52 C52 C2F 117.1(8) . . ?
N52 C52 H52 121.4 . . ?
C2F C52 H52 121.4 . . ?
C6F N1F C2F 116.4(8) . . ?
C6F N1F Re1 127.5(6) . . ?
C2F N1F Re1 116.0(6) . . ?
C3F C2F N1F 123.5(8) . . ?
C3F C2F C52 122.3(8) . . ?
N1F C2F C52 114.2(8) . . ?
C2F C3F C4F 119.7(9) . . ?
C2F C3F H3F 120.1 . . ?
C4F C3F H3F 120.1 . . ?
C5F C4F C3F 117.2(9) . . ?
C5F C4F H4F 121.4 . . ?
C3F C4F H4F 121.4 . . ?
C6F C5F C4F 120.8(9) . . ?
C6F C5F H5F 119.6 . . ?
C4F C5F H5F 119.6 . . ?
N1F C6F C5F 122.3(8) . . ?
N1F C6F H6F 118.9 . . ?
C5F C6F H6F 118.9 . . ?
O1S S1S C12S 105.7(4) . . ?
O1S S1S C11S 106.8(5) . . ?
C12S S1S C11S 96.6(5) . . ?
S1S C11S H11A 109.5 . . ?
S1S C11S H11B 109.5 . . ?
H11A C11S H11B 109.5 . . ?
S1S C11S H11C 109.5 . . ?
H11A C11S H11C 109.5 . . ?
H11B C11S H11C 109.5 . . ?
S1S C12S H12A 109.5 . . ?
S1S C12S H12B 109.5 . . ?
H12A C12S H12B 109.5 . . ?
S1S C12S H12C 109.5 . . ?
H12A C12S H12C 109.5 . . ?
H12B C12S H12C 109.5 . . ?
O2S S2S C21S 106.9(4) . . ?
O2S S2S C22S 106.4(4) . . ?
C21S S2S C22S 98.9(5) . . ?
S2S C21S H21A 109.5 . . ?
S2S C21S H21B 109.5 . . ?
H21A C21S H21B 109.5 . . ?
S2S C21S H21C 109.5 . . ?
H21A C21S H21C 109.5 . . ?
H21B C21S H21C 109.5 . . ?
S2S C22S H22A 109.5 . . ?
S2S C22S H22B 109.5 . . ?
H22A C22S H22B 109.5 . . ?
S2S C22S H22C 109.5 . . ?
H22A C22S H22C 109.5 . . ?
H22B C22S H22C 109.5 . . ?

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
O1W H11W O1S 0.848(10) 1.77(4) 2.584(9) 160(10) .
O1W H12W O2S 0.850(10) 1.84(3) 2.673(9) 165(9) .

_refine_diff_density_max         5.172
_refine_diff_density_min         -2.013
_refine_diff_density_rms         0.279

####################################################################### 
# 
# 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_fhre2090
_database_code_depnum_ccdc_archive 'CCDC 1457866'
_audit_update_record             
;
2016-07-07 deposited with the CCDC.
2016-08-16 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         'C21 H19 N7 O5 Re 1+, Cl O4 1-, C H2 Cl2'
_chemical_formula_sum            'C22 H21 Cl3 N7 O9 Re'
_chemical_formula_weight         820.01

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'
Cl Cl 0.1484 0.1585 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_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'
'-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                   13.949(4)
_cell_length_b                   16.578(4)
_cell_length_c                   25.764(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5958(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    106
_cell_measurement_theta_min      4
_cell_measurement_theta_max      20

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_F_000             3200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    4.408
_shelx_estimated_absorpt_T_min   0.177
_shelx_estimated_absorpt_T_max   0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.292
_exptl_absorpt_correction_T_max  0.667
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_number            41608
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.044
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6833
_reflns_number_gt                4801
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1000P)²+65.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6833
_refine_ls_number_parameters     416
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0704
_refine_ls_wR_factor_ref         0.2076
_refine_ls_wR_factor_gt          0.1867
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_restrained_S_all      1.162
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Re Re 0.67147(3) 0.31670(2) 0.54781(2) 0.02144(15) Uani 1 1 d . . . . .
C7X C 0.7516(7) 0.4111(7) 0.5514(4) 0.029(2) Uani 1 1 d . . . . .
O7X O 0.7980(6) 0.4692(5) 0.5551(3) 0.040(2) Uani 1 1 d . . . . .
C8X C 0.7572(8) 0.2727(6) 0.4956(4) 0.027(2) Uani 1 1 d . . . . .
O8X O 0.8097(6) 0.2480(5) 0.4654(3) 0.0365(19) Uani 1 1 d . . . . .
C9X C 0.7528(9) 0.2610(7) 0.5964(4) 0.032(2) Uani 1 1 d . . . . .
O9X O 0.7992(7) 0.2235(6) 0.6237(3) 0.044(2) Uani 1 1 d . . . . .
N1 N 0.5452(7) 0.3454(9) 0.8158(4) 0.058(4) Uani 1 1 d . . . . .
C1 C 0.4622(10) 0.365(2) 0.8487(6) 0.130(12) Uani 1 1 d . . . . .
H1A H 0.4762 0.3511 0.8840 0.195 Uiso 1 1 d R U . . .
H1B H 0.4074 0.3356 0.8369 0.195 Uiso 1 1 d R U . . .
H1C H 0.4489 0.4221 0.8467 0.195 Uiso 1 1 d R U . . .
C2 C 0.6266(10) 0.3164(9) 0.8395(5) 0.045(3) Uani 1 1 d . . . . .
O2 O 0.6258(8) 0.2977(7) 0.8853(3) 0.062(3) Uani 1 1 d . . . . .
N3 N 0.7066(8) 0.3060(6) 0.8092(4) 0.032(2) Uani 1 1 d . . . . .
C3 C 0.7930(10) 0.2776(8) 0.8354(5) 0.041(3) Uani 1 1 d . . . . .
H3A H 0.7789 0.2682 0.8713 0.062 Uiso 1 1 d R U . . .
H3B H 0.8427 0.3173 0.8325 0.062 Uiso 1 1 d R U . . .
H3C H 0.8139 0.2282 0.8196 0.062 Uiso 1 1 d R U . . .
C4 C 0.7101(10) 0.3257(7) 0.7569(4) 0.035(3) Uani 1 1 d . . . . .
O4 O 0.7856(6) 0.3163(5) 0.7327(3) 0.0364(19) Uani 1 1 d . . . . .
C5 C 0.6214(8) 0.3537(7) 0.7327(4) 0.030(2) Uani 1 1 d . . . . .
C6 C 0.5418(9) 0.3641(11) 0.7635(5) 0.049(4) Uani 1 1 d . . . . .
N6 N 0.4617(7) 0.3953(11) 0.7438(4) 0.079(6) Uani 1 1 d . . . . .
H6A H 0.4598 0.4095 0.7117 0.095 Uiso 1 1 d R U . . .
H6B H 0.4120 0.4015 0.7632 0.095 Uiso 1 1 d R U . . .
C51 C 0.6229(8) 0.3581(7) 0.6779(4) 0.029(2) Uani 1 1 d . . . . .
H51 H 0.6799 0.3468 0.6606 0.035 Uiso 1 1 d R U . . .
N51 N 0.5479(7) 0.3772(6) 0.6505(4) 0.031(2) Uani 1 1 d . . . . .
N52 N 0.5584(6) 0.3703(5) 0.5970(3) 0.0217(17) Uani 1 1 d . . . . .
C52 C 0.4826(7) 0.3959(6) 0.5730(4) 0.025(2) Uani 1 1 d . . . . .
H52 H 0.4296 0.4149 0.5912 0.030 Uiso 1 1 d R U . . .
N1F N 0.5665(6) 0.3669(5) 0.4937(3) 0.0222(18) Uani 1 1 d . . . . .
C2F C 0.4834(7) 0.3938(6) 0.5160(4) 0.023(2) Uani 1 1 d . . . . .
C3F C 0.4066(8) 0.4200(6) 0.4869(4) 0.026(2) Uani 1 1 d . . . . .
H3F H 0.3508 0.4381 0.5029 0.031 Uiso 1 1 d R U . . .
C4F C 0.4144(9) 0.4188(6) 0.4326(4) 0.030(2) Uani 1 1 d . . . . .
H4F H 0.3637 0.4352 0.4117 0.036 Uiso 1 1 d R U . . .
C5F C 0.5001(8) 0.3924(7) 0.4107(4) 0.031(2) Uani 1 1 d . . . . .
H5F H 0.5073 0.3921 0.3749 0.037 Uiso 1 1 d R U . . .
C6F C 0.5741(8) 0.3668(7) 0.4418(4) 0.029(2) Uani 1 1 d . . . . .
H6F H 0.6307 0.3490 0.4265 0.035 Uiso 1 1 d R U . . .
N1P N 0.5730(7) 0.2119(5) 0.5474(3) 0.0267(19) Uani 1 1 d . . . . .
C2P C 0.5337(8) 0.1857(7) 0.5917(5) 0.032(2) Uani 1 1 d . . . . .
H2P H 0.5494 0.2118 0.6225 0.039 Uiso 1 1 d R U . . .
C3P C 0.4706(8) 0.1215(7) 0.5935(5) 0.036(3) Uani 1 1 d . . . . .
H3P H 0.4450 0.1047 0.6251 0.044 Uiso 1 1 d R U . . .
C4P C 0.4456(8) 0.0822(7) 0.5480(5) 0.034(3) Uani 1 1 d . . . . .
H4P H 0.4015 0.0402 0.5477 0.041 Uiso 1 1 d R U . . .
C5P C 0.4893(9) 0.1085(7) 0.5028(5) 0.036(3) Uani 1 1 d . . . . .
H5P H 0.4769 0.0817 0.4718 0.043 Uiso 1 1 d R U . . .
C6P C 0.5515(8) 0.1740(6) 0.5027(5) 0.029(2) Uani 1 1 d . . . . .
H6P H 0.5782 0.1918 0.4717 0.035 Uiso 1 1 d R U . . .
Cl Cl 0.7409(2) 0.01130(17) 0.86159(12) 0.0420(7) Uani 1 1 d . . . . .
O1P O 0.8337(7) -0.0108(7) 0.8446(4) 0.061(3) Uani 1 1 d . . . . .
O2P O 0.6708(7) -0.0320(6) 0.8326(4) 0.054(3) Uani 1 1 d . . . . .
O3P O 0.7274(7) -0.0057(7) 0.9149(4) 0.054(3) Uani 1 1 d . . . . .
O4P O 0.7247(11) 0.0967(6) 0.8539(5) 0.086(4) Uani 1 1 d . . . . .
Cl1D Cl 0.2088(9) 0.4590(6) 0.3260(4) 0.040(2) Uani 0.3 1 d D . P A 1
Cl2D Cl 0.3883(10) 0.4105(9) 0.2746(5) 0.051(3) Uani 0.3 1 d D . P A 1
C1D C 0.3230(19) 0.4877(16) 0.305(2) 0.060 Uiso 0.3 1 d D U P A 1
H1D H 0.3584 0.5033 0.3359 0.090 Uiso 0.3 1 d R U P A 1
H2D H 0.3182 0.5349 0.2831 0.090 Uiso 0.3 1 d R U P A 1
Cl3D Cl 0.4935(11) 0.3353(8) 0.2394(6) 0.048(3) Uani 0.28 1 d D . P B 2
Cl4D Cl 0.3744(11) 0.4470(7) 0.2970(6) 0.050(3) Uani 0.28 1 d D . P B 2
C2D C 0.3752(14) 0.363(2) 0.255(2) 0.060 Uiso 0.28 1 d D U P B 2
H3D H 0.3393 0.3748 0.2241 0.090 Uiso 0.28 1 d R U P B 2
H4D H 0.3444 0.3180 0.2728 0.090 Uiso 0.28 1 d R U P B 2
Cl5D Cl 0.1058(9) 0.3643(8) 0.2673(5) 0.040(3) Uiso 0.24 1 d D . P C 3
Cl6D Cl 0.2551(13) 0.4638(11) 0.3107(7) 0.053(4) Uiso 0.24 1 d D . P C 3
C3D C 0.2305(12) 0.381(3) 0.270(2) 0.060 Uiso 0.24 1 d D U P C 3
H5D H 0.2633 0.3340 0.2832 0.090 Uiso 0.24 1 d R U P C 3
H6D H 0.2553 0.3929 0.2357 0.090 Uiso 0.24 1 d R U P C 3
Cl7D Cl 0.4814(16) 0.3312(14) 0.2604(9) 0.040(5) Uiso 0.18 1 d D . P D 4
Cl8D Cl 0.6234(17) 0.4304(16) 0.2023(9) 0.069(6) Uiso 0.18 1 d D . P D 4
C4D C 0.526(4) 0.4279(18) 0.246(3) 0.060 Uiso 0.18 1 d D U P D 4
H7D H 0.5454 0.4536 0.2779 0.090 Uiso 0.18 1 d R U P D 4
H8D H 0.4743 0.4597 0.2311 0.090 Uiso 0.18 1 d R U P D 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re C9X 1.924(12) . ?
Re C7X 1.925(12) . ?
Re C8X 1.942(12) . ?
Re N1F 2.185(8) . ?
Re N52 2.210(8) . ?
Re N1P 2.214(9) . ?
C7X O7X 1.163(14) . ?
C8X O8X 1.145(13) . ?
C9X O9X 1.141(14) . ?
N1 C2 1.377(19) . ?
N1 C6 1.382(16) . ?
N1 C1 1.473(19) . ?
C1 H1A 0.9598 . ?
C1 H1B 0.9602 . ?
C1 H1C 0.9599 . ?
C2 O2 1.220(15) . ?
C2 N3 1.372(17) . ?
N3 C4 1.386(14) . ?
N3 C3 1.459(16) . ?
C3 H3A 0.9599 . ?
C3 H3B 0.9601 . ?
C3 H3C 0.9602 . ?
C4 O4 1.234(15) . ?
C4 C5 1.461(18) . ?
C5 C6 1.375(16) . ?
C5 C51 1.416(15) . ?
C6 N6 1.332(18) . ?
N6 H6A 0.8599 . ?
N6 H6B 0.8600 . ?
C51 N51 1.301(14) . ?
C51 H51 0.9300 . ?
N51 N52 1.390(12) . ?
N52 C52 1.296(13) . ?
C52 C2F 1.469(14) . ?
C52 H52 0.9300 . ?
N1F C6F 1.342(13) . ?
N1F C2F 1.369(13) . ?
C2F C3F 1.379(14) . ?
C3F C4F 1.405(15) . ?
C3F H3F 0.9300 . ?
C4F C5F 1.392(15) . ?
C4F H4F 0.9299 . ?
C5F C6F 1.373(15) . ?
C5F H5F 0.9300 . ?
C6F H6F 0.9300 . ?
N1P C2P 1.340(14) . ?
N1P C6P 1.345(14) . ?
C2P C3P 1.382(16) . ?
C2P H2P 0.9303 . ?
C3P C4P 1.387(17) . ?
C3P H3P 0.9298 . ?
C4P C5P 1.384(17) . ?
C4P H4P 0.9301 . ?
C5P C6P 1.389(15) . ?
C5P H5P 0.9303 . ?
C6P H6P 0.9298 . ?
Cl O1P 1.414(10) . ?
Cl O3P 1.415(9) . ?
Cl O2P 1.424(10) . ?
Cl O4P 1.448(11) . ?
Cl1D C1D 1.748(10) . ?
Cl2D C1D 1.757(10) . ?
C1D H1D 0.9702 . ?
C1D H2D 0.9697 . ?
Cl3D C2D 1.762(10) . ?
Cl4D C2D 1.757(10) . ?
C2D H3D 0.9699 . ?
C2D H4D 0.9698 . ?
Cl5D C3D 1.765(10) . ?
Cl6D C3D 1.755(10) . ?
C3D H5D 0.9698 . ?
C3D H6D 0.9699 . ?
Cl7D C4D 1.759(10) . ?
Cl8D C4D 1.761(10) . ?
C4D H7D 0.9703 . ?
C4D H8D 0.9698 . ?

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
C9X Re C7X 91.0(5) . . ?
C9X Re C8X 84.7(4) . . ?
C7X Re C8X 88.9(4) . . ?
C9X Re N1F 172.6(4) . . ?
C7X Re N1F 96.3(4) . . ?
C8X Re N1F 96.5(4) . . ?
C9X Re N52 103.9(4) . . ?
C7X Re N52 93.4(4) . . ?
C8X Re N52 171.0(4) . . ?
N1F Re N52 74.6(3) . . ?
C9X Re N1P 89.6(4) . . ?
C7X Re N1P 176.3(4) . . ?
C8X Re N1P 94.8(4) . . ?
N1F Re N1P 83.1(3) . . ?
N52 Re N1P 82.9(3) . . ?
O7X C7X Re 177.5(9) . . ?
O8X C8X Re 178.1(10) . . ?
O9X C9X Re 175.7(11) . . ?
C2 N1 C6 122.5(11) . . ?
C2 N1 C1 118.1(11) . . ?
C6 N1 C1 119.0(13) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.1 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 110.0 . . ?
H1A C1 H1C 109.4 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 N3 121.8(14) . . ?
O2 C2 N1 120.6(13) . . ?
N3 C2 N1 117.5(11) . . ?
C2 N3 C4 123.5(11) . . ?
C2 N3 C3 116.6(10) . . ?
C4 N3 C3 119.8(11) . . ?
N3 C3 H3A 109.3 . . ?
N3 C3 H3B 109.8 . . ?
H3A C3 H3B 109.4 . . ?
N3 C3 H3C 109.3 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 N3 119.4(12) . . ?
O4 C4 C5 123.2(10) . . ?
N3 C4 C5 117.4(11) . . ?
C6 C5 C51 125.6(11) . . ?
C6 C5 C4 118.5(10) . . ?
C51 C5 C4 115.4(10) . . ?
N6 C6 C5 120.4(11) . . ?
N6 C6 N1 119.1(11) . . ?
C5 C6 N1 120.4(12) . . ?
C6 N6 H6A 119.9 . . ?
C6 N6 H6B 120.1 . . ?
H6A N6 H6B 120.0 . . ?
N51 C51 C5 122.8(10) . . ?
N51 C51 H51 118.4 . . ?
C5 C51 H51 118.8 . . ?
C51 N51 N52 115.6(9) . . ?
C52 N52 N51 111.0(8) . . ?
C52 N52 Re 116.1(7) . . ?
N51 N52 Re 132.6(6) . . ?
N52 C52 C2F 117.5(9) . . ?
N52 C52 H52 121.3 . . ?
C2F C52 H52 121.2 . . ?
C6F N1F C2F 119.0(9) . . ?
C6F N1F Re 125.7(7) . . ?
C2F N1F Re 115.1(6) . . ?
N1F C2F C3F 122.2(9) . . ?
N1F C2F C52 115.7(9) . . ?
C3F C2F C52 122.0(9) . . ?
C2F C3F C4F 118.5(10) . . ?
C2F C3F H3F 120.7 . . ?
C4F C3F H3F 120.8 . . ?
C5F C4F C3F 118.3(10) . . ?
C5F C4F H4F 120.8 . . ?
C3F C4F H4F 120.8 . . ?
C6F C5F C4F 120.5(10) . . ?
C6F C5F H5F 119.8 . . ?
C4F C5F H5F 119.8 . . ?
N1F C6F C5F 121.5(10) . . ?
N1F C6F H6F 119.3 . . ?
C5F C6F H6F 119.2 . . ?
C2P N1P C6P 119.1(10) . . ?
C2P N1P Re 120.3(7) . . ?
C6P N1P Re 120.6(7) . . ?
N1P C2P C3P 122.7(11) . . ?
N1P C2P H2P 118.7 . . ?
C3P C2P H2P 118.6 . . ?
C2P C3P C4P 119.5(12) . . ?
C2P C3P H3P 120.3 . . ?
C4P C3P H3P 120.2 . . ?
C5P C4P C3P 116.9(11) . . ?
C5P C4P H4P 121.5 . . ?
C3P C4P H4P 121.6 . . ?
C4P C5P C6P 121.6(11) . . ?
C4P C5P H5P 119.2 . . ?
C6P C5P H5P 119.2 . . ?
N1P C6P C5P 120.2(11) . . ?
N1P C6P H6P 119.9 . . ?
C5P C6P H6P 119.9 . . ?
O1P Cl O3P 111.8(7) . . ?
O1P Cl O2P 109.6(6) . . ?
O3P Cl O2P 108.5(6) . . ?
O1P Cl O4P 110.7(7) . . ?
O3P Cl O4P 107.8(7) . . ?
O2P Cl O4P 108.3(8) . . ?
Cl1D C1D Cl2D 114.3(13) . . ?
Cl1D C1D H1D 106.5 . . ?
Cl2D C1D H1D 107.3 . . ?
Cl1D C1D H2D 109.7 . . ?
Cl2D C1D H2D 111.2 . . ?
H1D C1D H2D 107.4 . . ?
Cl4D C2D Cl3D 110.8(14) . . ?
Cl4D C2D H3D 110.0 . . ?
Cl3D C2D H3D 109.9 . . ?
Cl4D C2D H4D 109.0 . . ?
Cl3D C2D H4D 108.9 . . ?
H3D C2D H4D 108.1 . . ?
Cl6D C3D Cl5D 109.9(14) . . ?
Cl6D C3D H5D 109.3 . . ?
Cl5D C3D H5D 110.4 . . ?
Cl6D C3D H6D 108.7 . . ?
Cl5D C3D H6D 110.3 . . ?
H5D C3D H6D 108.2 . . ?
Cl7D C4D Cl8D 115(2) . . ?
Cl7D C4D H7D 108.5 . . ?
Cl8D C4D H7D 108.4 . . ?
Cl7D C4D H8D 108.5 . . ?
Cl8D C4D H8D 108.2 . . ?
H7D C4D H8D 107.5 . . ?

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
N6 H6A N51 0.86 2.07 2.706(14) 130.1 .
N6 H6B O4 0.86 2.26 2.848(15) 125.5 6_557

_refine_diff_density_max         4.498
_refine_diff_density_min         -3.363
_refine_diff_density_rms         0.265

####################################################################### 
# 
# 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_hexafp
_database_code_depnum_ccdc_archive 'CCDC 1457867'
_audit_update_record             
;
2016-03-04 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H19 N7 O5 Re 1+, F6 P 1-, C H4 O'
_chemical_formula_sum            'C22 H23 F6 N7 O6 P Re'
_chemical_formula_weight         812.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   8.1340(16)
_cell_length_b                   13.116(3)
_cell_length_c                   14.260(3)
_cell_angle_alpha                73.28(3)
_cell_angle_beta                 74.05(3)
_cell_angle_gamma                76.64(3)
_cell_volume                     1381.7(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    175
_cell_measurement_theta_min      4
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_F_000             792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    4.548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.284
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_number            37695
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_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         2.641
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6347
_reflns_number_gt                5028
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.1000P)²+0.2500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6347
_refine_ls_number_parameters     376
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1537
_refine_ls_wR_factor_gt          0.1282
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         3.888
_refine_diff_density_min         -2.396
_refine_diff_density_rms         0.307

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
Re Re 0.17858(3) 0.26389(2) 0.33932(2) 0.02583(13) Uani 1 1 d . . . . .
C7X C -0.0312(10) 0.3348(6) 0.2921(7) 0.0335(17) Uani 1 1 d . . . . .
O7X O -0.1622(8) 0.3690(5) 0.2712(6) 0.060(2) Uani 1 1 d . . . . .
C8X C 0.0295(11) 0.2270(7) 0.4711(7) 0.0355(18) Uani 1 1 d . . . . .
O8X O -0.0631(9) 0.2060(6) 0.5460(5) 0.0560(19) Uani 1 1 d . . . . .
C9X C 0.1391(9) 0.1307(6) 0.3251(5) 0.0286(16) Uani 1 1 d . . . . .
O9X O 0.1121(7) 0.0488(4) 0.3230(4) 0.0339(12) Uani 1 1 d . . . . .
N1 N 0.5711(8) 0.1423(5) -0.1428(4) 0.026 Uani 1 1 d . . . . .
C1 C 0.7279(10) 0.1586(6) -0.2218(6) 0.0313(17) Uani 1 1 d . . . . .
H1A H 0.7387 0.2342 -0.2438 0.047 Uiso 1 1 d R U . . .
H1B H 0.7241 0.1341 -0.2789 0.047 Uiso 1 1 d R U . . .
H1C H 0.8288 0.1181 -0.1967 0.047 Uiso 1 1 d R U . . .
C2 C 0.4724(9) 0.0727(6) -0.1503(5) 0.027 Uani 1 1 d . . . . .
O2 O 0.5111(7) 0.0288(4) -0.2197(4) 0.0332(12) Uani 1 1 d . . . . .
N3 N 0.3284(8) 0.0552(5) -0.0738(5) 0.027 Uani 1 1 d . . . . .
C3 C 0.2229(11) -0.0167(7) -0.0829(7) 0.0375(19) Uani 1 1 d . . . . .
H3A H 0.1510 -0.0438 -0.0183 0.056 Uiso 1 1 d R U . . .
H3B H 0.2971 -0.0765 -0.1075 0.056 Uiso 1 1 d R U . . .
H3C H 0.1502 0.0224 -0.1291 0.056 Uiso 1 1 d R U . . .
C4 C 0.2715(10) 0.1069(6) 0.0053(6) 0.0286(16) Uani 1 1 d . . . . .
O4 O 0.1375(7) 0.0868(5) 0.0689(4) 0.0420(14) Uani 1 1 d . . . . .
C5 C 0.3821(11) 0.1786(7) 0.0077(6) 0.0342(19) Uani 1 1 d . . . . .
C6 C 0.5239(11) 0.1944(7) -0.0651(6) 0.0376(16) Uani 1 1 d . . . . .
N6 N 0.6288(9) 0.2616(6) -0.0697(5) 0.0427(18) Uani 1 1 d . . . . .
H61 H 0.6056 0.2973 -0.0243 0.051 Uiso 1 1 d R U . . .
H62 H 0.7188 0.2695 -0.1181 0.051 Uiso 1 1 d R U . . .
C51 C 0.3317(9) 0.2229(6) 0.0928(5) 0.0261(15) Uani 1 1 d . . . . .
H51 H 0.2328 0.2056 0.1412 0.031 Uiso 1 1 d R U . . .
N51 N 0.4183(8) 0.2868(5) 0.1066(5) 0.0293(14) Uani 1 1 d . . . . .
N52 N 0.3580(8) 0.3216(5) 0.1950(5) 0.0252(13) Uani 1 1 d . . . . .
C52 C 0.4307(10) 0.4008(6) 0.1942(6) 0.0306(16) Uani 1 1 d . . . . .
H52 H 0.5126 0.4278 0.1379 0.037 Uiso 1 1 d R U . . .
N1F N 0.2571(8) 0.4037(5) 0.3572(4) 0.0239(12) Uani 1 1 d . . . . .
C2F C 0.3842(10) 0.4464(6) 0.2803(5) 0.0259(15) Uani 1 1 d . . . . .
C3F C 0.4644(10) 0.5263(6) 0.2859(6) 0.0312(16) Uani 1 1 d . . . . .
H3F H 0.5524 0.5525 0.2333 0.037 Uiso 1 1 d R U . . .
C4F C 0.4126(10) 0.5658(7) 0.3711(6) 0.0343(18) Uani 1 1 d . . . . .
H4F H 0.4630 0.6205 0.3759 0.041 Uiso 1 1 d R U . . .
C5F C 0.2854(10) 0.5245(6) 0.4481(6) 0.0311(16) Uani 1 1 d . . . . .
H5F H 0.2484 0.5499 0.5063 0.037 Uiso 1 1 d R U . . .
C6F C 0.2113(9) 0.4433(6) 0.4380(6) 0.0287(16) Uani 1 1 d . . . . .
H6F H 0.1249 0.4155 0.4909 0.034 Uiso 1 1 d R U . . .
N1P N 0.4181(8) 0.1830(5) 0.3913(4) 0.0238(12) Uani 1 1 d . . . . .
C2P C 0.5514(10) 0.1301(6) 0.3339(6) 0.0282(15) Uani 1 1 d . . . . .
H2P H 0.5415 0.1292 0.2707 0.034 Uiso 1 1 d R U . . .
C3P C 0.7011(10) 0.0778(7) 0.3652(6) 0.0351(18) Uani 1 1 d . . . . .
H3P H 0.7925 0.0452 0.3222 0.042 Uiso 1 1 d R U . . .
C4P C 0.7152(10) 0.0731(6) 0.4598(6) 0.0352(18) Uani 1 1 d . . . . .
H4P H 0.8148 0.0361 0.4823 0.042 Uiso 1 1 d R U . . .
C5P C 0.5767(11) 0.1253(7) 0.5229(7) 0.0372(19) Uani 1 1 d . . . . .
H5P H 0.5821 0.1240 0.5875 0.045 Uiso 1 1 d R U . . .
C6P C 0.4342(10) 0.1781(6) 0.4851(6) 0.0314(17) Uani 1 1 d . . . . .
H6P H 0.3422 0.2128 0.5262 0.038 Uiso 1 1 d R U . . .
P P 0.1102(3) 0.32842(17) 0.75315(16) 0.0325(5) Uani 1 1 d . . . . .
F1 F 0.1703(8) 0.4301(4) 0.6702(4) 0.0525(14) Uani 1 1 d . . . . .
F2 F 0.0478(8) 0.2269(5) 0.8376(5) 0.0642(18) Uani 1 1 d . . . . .
F3 F 0.2925(10) 0.2614(6) 0.7176(7) 0.111(3) Uani 1 1 d . . . . .
F4 F 0.0416(12) 0.2991(8) 0.6729(5) 0.118(4) Uani 1 1 d . . . . .
F5 F -0.0719(10) 0.3930(7) 0.7858(6) 0.122(4) Uani 1 1 d . . . . .
F6 F 0.1896(12) 0.3535(7) 0.8307(5) 0.107(3) Uani 1 1 d . . . . .
O1M O 0.770(2) 0.4162(11) 0.0007(12) 0.071(4) Uiso 0.5 1 d D . P A 1
H1M H 0.8134 0.4099 -0.0584 0.085 Uiso 0.5 1 d R U P A 1
C1M C 0.852(3) 0.3169(14) 0.0581(14) 0.046(4) Uiso 0.5 1 d D . P A 1
H11M H 0.9222 0.3336 0.0943 0.055 Uiso 0.5 1 d R U P A 1
H12M H 0.9239 0.2727 0.0141 0.055 Uiso 0.5 1 d R U P A 1
H13M H 0.7639 0.2787 0.1048 0.055 Uiso 0.5 1 d R U P A 1
O2M O 0.852(4) 0.253(2) 0.106(2) 0.074(8) Uiso 0.27 1 d D . P B 2
H2M H 0.9201 0.1974 0.0942 0.089 Uiso 0.27 1 d R U P B 2
C2M C 0.899(7) 0.357(3) 0.052(4) 0.081(15) Uiso 0.27 1 d D . P B 2
H21M H 0.8045 0.4117 0.0711 0.097 Uiso 0.27 1 d R U P B 2
H22M H 0.9196 0.3637 -0.0191 0.097 Uiso 0.27 1 d R U P B 2
H23M H 1.0013 0.3659 0.0678 0.097 Uiso 0.27 1 d R U P B 2
O3M O 1.015(4) 0.424(3) 0.013(3) 0.081(10) Uiso 0.23 1 d D . P C 3
H3M H 1.0659 0.4039 -0.0400 0.097 Uiso 0.23 1 d R U P C 3
C3M C 0.864(5) 0.500(3) -0.007(3) 0.056(11) Uiso 0.23 1 d D . P C 3
H31M H 0.7871 0.5103 0.0555 0.067 Uiso 0.23 1 d R U P C 3
H32M H 0.8062 0.4728 -0.0424 0.067 Uiso 0.23 1 d R U P C 3
H33M H 0.8962 0.5682 -0.0469 0.067 Uiso 0.23 1 d R U P C 3


_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
Re C9X 1.922(8) . ?
Re C8X 1.932(9) . ?
Re C7X 1.941(8) . ?
Re N1F 2.177(6) . ?
Re N1P 2.204(6) . ?
Re N52 2.214(6) . ?
C7X O7X 1.141(10) . ?
C8X O8X 1.126(10) . ?
C9X O9X 1.156(9) . ?
N1 C2 1.390(9) . ?
N1 C1 1.462(9) . ?
N1 C6 1.387(10) . ?
C1 H1A 0.9677 . ?
C1 H1B 0.9676 . ?
C1 H1C 0.9673 . ?
C2 O2 1.217(9) . ?
C2 N3 1.376(10) . ?
N3 C4 1.398(10) . ?
N3 C3 1.465(9) . ?
C3 H3A 0.9632 . ?
C3 H3B 0.9632 . ?
C3 H3C 0.9631 . ?
C4 O4 1.238(9) . ?
C4 C5 1.457(11) . ?
C5 C6 1.334(12) . ?
C5 C51 1.413(10) . ?
C6 N6 1.339(10) . ?
N6 H61 0.8600 . ?
N6 H62 0.8600 . ?
C51 N51 1.297(9) . ?
C51 H51 0.9300 . ?
N51 N52 1.387(9) . ?
N52 C52 1.305(9) . ?
C52 C2F 1.439(10) . ?
C52 H52 0.9300 . ?
N1F C6F 1.325(9) . ?
N1F C2F 1.370(9) . ?
C2F C3F 1.387(10) . ?
C3F C4F 1.379(11) . ?
C3F H3F 0.9300 . ?
C4F C5F 1.365(11) . ?
C4F H4F 0.9300 . ?
C5F C6F 1.397(10) . ?
C5F H5F 0.9300 . ?
C6F H6F 0.9300 . ?
N1P C2P 1.348(9) . ?
N1P C6P 1.361(10) . ?
C2P C3P 1.375(10) . ?
C2P H2P 0.9300 . ?
C3P C4P 1.367(12) . ?
C3P H3P 0.9300 . ?
C4P C5P 1.410(12) . ?
C4P H4P 0.9300 . ?
C5P C6P 1.368(11) . ?
C5P H5P 0.9300 . ?
C6P H6P 0.9300 . ?
P F5 1.548(7) . ?
P F6 1.565(6) . ?
P F3 1.571(7) . ?
P F4 1.572(7) . ?
P F1 1.579(5) . ?
P F2 1.592(5) . ?
O1M C1M 1.449(10) . ?
O1M H1M 0.8400 . ?
C1M H11M 0.9600 . ?
C1M H12M 0.9600 . ?
C1M H13M 0.9600 . ?
O2M C2M 1.439(10) . ?
O2M H2M 0.8401 . ?
C2M H21M 0.9600 . ?
C2M H22M 0.9600 . ?
C2M H23M 0.9600 . ?
O3M C3M 1.431(10) . ?
O3M C3M 1.52(5) 2_765 ?
O3M H3M 0.8400 . ?
C3M O3M 1.52(5) 2_765 ?
C3M H31M 0.9600 . ?
C3M H32M 0.9600 . ?
C3M H33M 0.9600 . ?

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
C9X Re C8X 84.4(3) . . ?
C9X Re C7X 88.2(3) . . ?
C8X Re C7X 86.6(4) . . ?
C9X Re N1F 172.5(2) . . ?
C8X Re N1F 97.8(3) . . ?
C7X Re N1F 99.1(3) . . ?
C9X Re N1P 91.6(3) . . ?
C8X Re N1P 94.0(3) . . ?
C7X Re N1P 179.4(3) . . ?
N1F Re N1P 81.2(2) . . ?
C9X Re N52 102.6(3) . . ?
C8X Re N52 172.8(3) . . ?
C7X Re N52 95.1(3) . . ?
N1F Re N52 75.1(2) . . ?
N1P Re N52 84.3(2) . . ?
O7X C7X Re 173.4(8) . . ?
O8X C8X Re 177.0(8) . . ?
O9X C9X Re 175.8(7) . . ?
C2 N1 C1 116.4(6) . . ?
C2 N1 C6 122.1(6) . . ?
C1 N1 C6 121.4(6) . . ?
N1 C1 H1A 110.5 . . ?
N1 C1 H1B 110.4 . . ?
H1A C1 H1B 108.7 . . ?
N1 C1 H1C 109.8 . . ?
H1A C1 H1C 108.8 . . ?
H1B C1 H1C 108.6 . . ?
O2 C2 N3 121.6(7) . . ?
O2 C2 N1 122.4(7) . . ?
N3 C2 N1 116.0(6) . . ?
C2 N3 C4 124.7(6) . . ?
C2 N3 C3 115.9(6) . . ?
C4 N3 C3 119.3(6) . . ?
N3 C3 H3A 110.0 . . ?
N3 C3 H3B 109.7 . . ?
H3A C3 H3B 109.1 . . ?
N3 C3 H3C 109.6 . . ?
H3A C3 H3C 109.2 . . ?
H3B C3 H3C 109.1 . . ?
O4 C4 N3 119.3(7) . . ?
O4 C4 C5 124.9(7) . . ?
N3 C4 C5 115.8(7) . . ?
C6 C5 C51 124.8(8) . . ?
C6 C5 C4 119.8(7) . . ?
C51 C5 C4 115.3(8) . . ?
C5 C6 N6 123.3(8) . . ?
C5 C6 N1 121.5(7) . . ?
N6 C6 N1 115.3(7) . . ?
C6 N6 H61 119.9 . . ?
C6 N6 H62 120.1 . . ?
H61 N6 H62 120.0 . . ?
N51 C51 C5 122.7(7) . . ?
N51 C51 H51 118.2 . . ?
C5 C51 H51 119.1 . . ?
C51 N51 N52 116.8(6) . . ?
C52 N52 N51 112.6(6) . . ?
C52 N52 Re 113.9(5) . . ?
N51 N52 Re 133.4(5) . . ?
N52 C52 C2F 120.0(7) . . ?
N52 C52 H52 119.9 . . ?
C2F C52 H52 120.0 . . ?
C6F N1F C2F 116.9(6) . . ?
C6F N1F Re 127.3(5) . . ?
C2F N1F Re 115.2(5) . . ?
N1F C2F C3F 122.3(7) . . ?
N1F C2F C52 115.1(6) . . ?
C3F C2F C52 122.6(7) . . ?
C4F C3F C2F 119.1(7) . . ?
C4F C3F H3F 120.5 . . ?
C2F C3F H3F 120.5 . . ?
C5F C4F C3F 119.2(7) . . ?
C5F C4F H4F 120.3 . . ?
C3F C4F H4F 120.5 . . ?
C4F C5F C6F 118.8(7) . . ?
C4F C5F H5F 120.8 . . ?
C6F C5F H5F 120.5 . . ?
N1F C6F C5F 123.7(7) . . ?
N1F C6F H6F 118.1 . . ?
C5F C6F H6F 118.3 . . ?
C2P N1P C6P 116.8(6) . . ?
C2P N1P Re 121.4(5) . . ?
C6P N1P Re 121.6(5) . . ?
N1P C2P C3P 122.5(7) . . ?
N1P C2P H2P 118.6 . . ?
C3P C2P H2P 118.9 . . ?
C4P C3P C2P 120.0(8) . . ?
C4P C3P H3P 120.0 . . ?
C2P C3P H3P 120.0 . . ?
C3P C4P C5P 119.0(7) . . ?
C3P C4P H4P 120.6 . . ?
C5P C4P H4P 120.4 . . ?
C6P C5P C4P 117.4(8) . . ?
C6P C5P H5P 121.3 . . ?
C4P C5P H5P 121.3 . . ?
N1P C6P C5P 124.2(8) . . ?
N1P C6P H6P 117.9 . . ?
C5P C6P H6P 117.9 . . ?
F5 P F6 94.9(6) . . ?
F5 P F3 178.0(6) . . ?
F6 P F3 87.1(6) . . ?
F5 P F4 88.7(6) . . ?
F6 P F4 176.4(6) . . ?
F3 P F4 89.3(6) . . ?
F5 P F1 91.7(4) . . ?
F6 P F1 91.5(3) . . ?
F3 P F1 88.5(4) . . ?
F4 P F1 88.3(4) . . ?
F5 P F2 87.7(4) . . ?
F6 P F2 88.2(3) . . ?
F3 P F2 92.2(4) . . ?
F4 P F2 92.0(4) . . ?
F1 P F2 179.3(4) . . ?
C1M O1M H1M 101.6 . . ?
O1M C1M H11M 109.4 . . ?
O1M C1M H12M 110.2 . . ?
H11M C1M H12M 109.5 . . ?
O1M C1M H13M 108.8 . . ?
H11M C1M H13M 109.5 . . ?
H12M C1M H13M 109.5 . . ?
C2M O2M H2M 118.9 . . ?
O2M C2M H21M 108.2 . . ?
O2M C2M H22M 109.9 . . ?
H21M C2M H22M 109.5 . . ?
O2M C2M H23M 110.3 . . ?
H21M C2M H23M 109.5 . . ?
H22M C2M H23M 109.5 . . ?
C3M O3M C3M 101(3) . 2_765 ?
C3M O3M H3M 107.6 . . ?
C3M O3M H3M 98.1 2_765 . ?
O3M C3M O3M 79(3) . 2_765 ?
O3M C3M H31M 109.5 . . ?
O3M C3M H31M 96.7 2_765 . ?
O3M C3M H32M 109.0 . . ?
O3M C3M H32M 147.1 2_765 . ?
H31M C3M H32M 109.5 . . ?
O3M C3M H33M 110.0 . . ?
O3M C3M H33M 40.7 2_765 . ?
H31M C3M H33M 109.5 . . ?
H32M C3M H33M 109.5 . . ?


_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_recoimin
_database_code_depnum_ccdc_archive 'CCDC 1457868'
_audit_update_record             
;
2016-07-07 deposited with the CCDC.
2016-08-16 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         'C15 H13 Cl N5 O5 Re, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C15.50 H14 Cl2 N5 O5 Re'
_chemical_formula_weight         607.42

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'
Cl Cl 0.1484 0.1585 '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           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.7068(10)
_cell_length_b                   10.7442(8)
_cell_length_c                   13.8605(9)
_cell_angle_alpha                90
_cell_angle_beta                 103.693(5)
_cell_angle_gamma                90
_cell_volume                     1983.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    75
_cell_measurement_theta_min      4
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_F_000             1164
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.05
0 -1 0 0.05
1 0 0 0.05
-1 0 0 0.05
0 0 1 0.1
0 0 -1 0.1

_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    6.435
_shelx_estimated_absorpt_T_min   0.319
_shelx_estimated_absorpt_T_max   0.565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3192
_exptl_absorpt_correction_T_max  0.5655
_exptl_absorpt_process_details   '(SADABS 2.10, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_reflns_number            28481
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.571
_diffrn_reflns_theta_max         27.823
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4547
_reflns_number_gt                3468
_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       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0550P)²+6.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4547
_refine_ls_number_parameters     262
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1089
_refine_ls_wR_factor_gt          0.0972
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Re Re 0.26485(2) 0.39419(2) 0.41913(2) 0.01899(10) Uani 1 1 d . . . . .
Cl Cl 0.21886(12) 0.28059(15) 0.55905(12) 0.0238(3) Uani 1 1 d . . . . .
C7X C 0.2957(5) 0.4921(7) 0.3145(5) 0.0287(16) Uani 1 1 d . . . . .
O7X O 0.3138(4) 0.5548(6) 0.2521(4) 0.0420(14) Uani 1 1 d . . . . .
C8X C 0.2762(5) 0.2446(7) 0.3463(5) 0.0226(14) Uani 1 1 d . . . . .
O8X O 0.2796(4) 0.1556(5) 0.3016(3) 0.0298(11) Uani 1 1 d . . . . .
C9X C 0.4050(5) 0.3793(6) 0.4827(5) 0.0235(14) Uani 1 1 d . . . . .
O9X O 0.4865(3) 0.3629(5) 0.5209(4) 0.0315(12) Uani 1 1 d . . . . .
N1 N 0.4267(4) 0.7147(5) 0.6689(4) 0.0212(12) Uani 1 1 d . . . . .
C1 C 0.4984(5) 0.6878(7) 0.7643(5) 0.0291(16) Uani 1 1 d . . . . .
H1A H 0.5426 0.7597 0.7842 0.044 Uiso 1 1 d R U . . .
H1B H 0.4614 0.6711 0.8154 0.044 Uiso 1 1 d R U . . .
H1C H 0.5388 0.6149 0.7567 0.044 Uiso 1 1 d R U . . .
C2 C 0.4317(5) 0.8325(6) 0.6269(5) 0.0204(13) Uani 1 1 d . . . . .
O2 O 0.4970(3) 0.9059(4) 0.6628(4) 0.0237(10) Uani 1 1 d . . . . .
N3 N 0.3595(4) 0.8611(5) 0.5428(4) 0.0201(11) Uani 1 1 d . . . . .
C3 C 0.3571(6) 0.9872(7) 0.5012(6) 0.0322(17) Uani 1 1 d . . . . .
H3A H 0.3020 0.9934 0.4417 0.048 Uiso 1 1 d R U . . .
H3B H 0.3469 1.0479 0.5506 0.048 Uiso 1 1 d R U . . .
H3C H 0.4209 1.0043 0.4835 0.048 Uiso 1 1 d R U . . .
C4 C 0.2825(5) 0.7783(6) 0.4948(4) 0.0211(13) Uani 1 1 d . U . . .
O4 O 0.2290(4) 0.8131(4) 0.4182(3) 0.0305(11) Uani 1 1 d . U . . .
C5 C 0.2868(5) 0.6581(6) 0.5393(5) 0.0189(13) Uani 1 1 d . . . . .
C6 C 0.3569(5) 0.6272(6) 0.6262(5) 0.0182(13) Uani 1 1 d . . . . .
N6 N 0.3591(4) 0.5170(5) 0.6704(4) 0.0231(12) Uani 1 1 d . . . . .
H6A H 0.4045 0.5017 0.7257 0.028 Uiso 1 1 d R U . . .
H6B H 0.3151 0.4593 0.6444 0.028 Uiso 1 1 d R U . . .
N52 N 0.2222(4) 0.5656(5) 0.4869(4) 0.0174(11) Uani 1 1 d . . . . .
C52 C 0.1285(5) 0.5960(6) 0.4572(5) 0.0205(13) Uani 1 1 d . . . . .
H51 H 0.1038 0.6712 0.4785 0.025 Uiso 1 1 d R U . . .
N1F N 0.1055(4) 0.4095(5) 0.3604(4) 0.0179(11) Uani 1 1 d . . . . .
C2F C 0.0616(5) 0.5106(6) 0.3897(4) 0.0193(13) Uani 1 1 d . . . . .
C3F C -0.0411(5) 0.5322(7) 0.3576(5) 0.0254(15) Uani 1 1 d . . . . .
H3F H -0.0712 0.6039 0.3784 0.030 Uiso 1 1 d R U . . .
C4F C -0.0978(5) 0.4466(7) 0.2945(5) 0.0300(16) Uani 1 1 d . . . . .
H4F H -0.1679 0.4596 0.2704 0.036 Uiso 1 1 d R U . . .
C5F C -0.0536(6) 0.3420(7) 0.2662(6) 0.0348(18) Uani 1 1 d . . . . .
H5F H -0.0928 0.2815 0.2241 0.042 Uiso 1 1 d R U . . .
C6F C 0.0478(5) 0.3268(7) 0.2998(5) 0.0286(16) Uani 1 1 d . . . . .
H6F H 0.0786 0.2554 0.2795 0.034 Uiso 1 1 d R U . . .
Cl1S Cl 0.0615(3) -0.0659(4) 0.5859(3) 0.0959(11) Uani 1 1 d . . . . .
C1S C 0.0581(13) 0.0096(17) 0.4780(14) 0.050(5) Uani 0.5 1 d . . P A -1
H1S H 0.0829 -0.0477 0.4332 0.060 Uiso 0.5 1 d R U P A -1
H2S H 0.1051 0.0808 0.4921 0.060 Uiso 0.5 1 d R U P A -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
Re C7X 1.918(8) . ?
Re C9X 1.921(7) . ?
Re C8X 1.923(7) . ?
Re N1F 2.149(5) . ?
Re N52 2.208(5) . ?
Re Cl 2.4954(16) . ?
C7X O7X 1.168(9) . ?
C8X O8X 1.146(8) . ?
C9X O9X 1.131(8) . ?
N1 C6 1.371(8) . ?
N1 C2 1.403(8) . ?
N1 C1 1.478(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O2 1.208(8) . ?
C2 N3 1.373(8) . ?
N3 C4 1.419(8) . ?
N3 C3 1.470(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 O4 1.199(7) . ?
C4 C5 1.427(9) . ?
C5 C6 1.392(8) . ?
C5 N52 1.413(8) . ?
C6 N6 1.331(8) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
N52 C52 1.294(8) . ?
C52 C2F 1.467(9) . ?
C52 H51 0.9500 . ?
N1F C6F 1.344(8) . ?
N1F C2F 1.349(8) . ?
C2F C3F 1.393(9) . ?
C3F C4F 1.375(10) . ?
C3F H3F 0.9500 . ?
C4F C5F 1.378(11) . ?
C4F H4F 0.9500 . ?
C5F C6F 1.367(10) . ?
C5F H5F 0.9500 . ?
C6F H6F 0.9500 . ?
Cl1S C1S 1.69(2) . ?
C1S Cl1S 1.775(19) 3_556 ?
C1S H1S 0.9900 . ?
C1S H2S 0.9900 . ?

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
C7X Re C9X 91.0(3) . . ?
C7X Re C8X 90.1(3) . . ?
C9X Re C8X 88.6(3) . . ?
C7X Re N1F 93.3(2) . . ?
C9X Re N1F 175.1(2) . . ?
C8X Re N1F 93.8(2) . . ?
C7X Re N52 89.6(2) . . ?
C9X Re N52 102.2(2) . . ?
C8X Re N52 169.2(2) . . ?
N1F Re N52 75.49(19) . . ?
C7X Re Cl 175.8(2) . . ?
C9X Re Cl 90.7(2) . . ?
C8X Re Cl 93.8(2) . . ?
N1F Re Cl 84.88(15) . . ?
N52 Re Cl 86.35(14) . . ?
O7X C7X Re 178.0(6) . . ?
O8X C8X Re 177.7(6) . . ?
O9X C9X Re 175.7(6) . . ?
C6 N1 C2 122.5(5) . . ?
C6 N1 C1 120.1(6) . . ?
C2 N1 C1 117.4(5) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.4 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 N3 121.2(6) . . ?
O2 C2 N1 121.5(6) . . ?
N3 C2 N1 117.2(5) . . ?
C2 N3 C4 124.4(5) . . ?
C2 N3 C3 118.9(5) . . ?
C4 N3 C3 116.7(5) . . ?
N3 C3 H3A 109.5 . . ?
N3 C3 H3B 109.4 . . ?
H3A C3 H3B 109.5 . . ?
N3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 N3 116.8(6) . . ?
O4 C4 C5 128.3(6) . . ?
N3 C4 C5 114.5(5) . . ?
C6 C5 N52 119.8(6) . . ?
C6 C5 C4 122.7(6) . . ?
N52 C5 C4 117.2(5) . . ?
N6 C6 N1 118.3(6) . . ?
N6 C6 C5 123.2(6) . . ?
N1 C6 C5 118.6(6) . . ?
C6 N6 H6A 120.0 . . ?
C6 N6 H6B 119.9 . . ?
H6A N6 H6B 120.0 . . ?
C52 N52 C5 116.1(5) . . ?
C52 N52 Re 114.7(4) . . ?
C5 N52 Re 127.5(4) . . ?
N52 C52 C2F 117.9(6) . . ?
N52 C52 H51 121.1 . . ?
C2F C52 H51 121.0 . . ?
C6F N1F C2F 118.8(5) . . ?
C6F N1F Re 125.5(4) . . ?
C2F N1F Re 115.6(4) . . ?
N1F C2F C3F 121.8(6) . . ?
N1F C2F C52 116.1(5) . . ?
C3F C2F C52 122.1(6) . . ?
C4F C3F C2F 117.9(7) . . ?
C4F C3F H3F 121.0 . . ?
C2F C3F H3F 121.1 . . ?
C3F C4F C5F 120.4(6) . . ?
C3F C4F H4F 119.9 . . ?
C5F C4F H4F 119.7 . . ?
C6F C5F C4F 118.7(7) . . ?
C6F C5F H5F 120.6 . . ?
C4F C5F H5F 120.7 . . ?
N1F C6F C5F 122.3(7) . . ?
N1F C6F H6F 118.8 . . ?
C5F C6F H6F 118.8 . . ?
Cl1S C1S Cl1S 115.7(10) . 3_556 ?
Cl1S C1S H1S 108.3 . . ?
Cl1S C1S H1S 108.3 3_556 . ?
Cl1S C1S H2S 108.4 . . ?
Cl1S C1S H2S 108.4 3_556 . ?
H1S C1S H2S 107.4 . . ?

_refine_diff_density_max         4.684
_refine_diff_density_min         -1.742
_refine_diff_density_rms         0.234

