# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_P17424
_database_code_depnum_ccdc_archive 'CCDC 2494313'
loop_
_audit_author_name
_audit_author_address
'Michael K. Takase'
;California Institute of Technology
United States of America
;
_audit_update_record             
;
2025-10-15 deposited with the CCDC.	2026-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21H28BrMnN4O32+ 2(F6P-) 0.3(H2O)'
_chemical_formula_sum            'C21 H28.67 Br F12 Mn N4 O3.33 P2'
_chemical_formula_weight         815.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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                   18.0875(14)
_cell_length_b                   13.3416(11)
_cell_length_c                   12.7322(9)
_cell_angle_alpha                90
_cell_angle_beta                 94.982(5)
_cell_angle_gamma                90
_cell_volume                     3060.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6316
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      74.26

_exptl_crystal_description       Block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_F_000             1629
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    7.024
_shelx_estimated_absorpt_T_min   0.540
_shelx_estimated_absorpt_T_max   0.720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            29184
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_av_R_equivalents  0.1328
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.452
_diffrn_reflns_theta_max         73.496
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6147
_reflns_number_gt                3942
_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       'APEX3 v2017.3-0 (Bruker-AXS, 2017)'
_computing_cell_refinement       'SAINT v8.38A (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT v8.38A (Bruker-AXS, 2013)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0536P)²+21.5707P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6147
_refine_ls_number_parameters     412
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0783
_refine_ls_wR_factor_ref         0.1913
_refine_ls_wR_factor_gt          0.1650
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.54845(5) 0.78560(8) 0.54608(7) 0.0453(3) Uani 1 1 d . . . . .
Mn1 Mn 0.61399(6) 0.70191(10) 0.70686(9) 0.0321(3) Uani 1 1 d . . . . .
N1 N 0.6187(3) 0.5708(5) 0.6232(5) 0.0314(14) Uani 1 1 d . . . . .
C1 C 0.5727(4) 0.4932(6) 0.6251(6) 0.0350(17) Uani 1 1 d . . . . .
H1 H 0.532344 0.497349 0.667956 0.042 Uiso 1 1 calc R U . . .
C2 C 0.5809(4) 0.4075(6) 0.5680(6) 0.0340(17) Uani 1 1 d . . . . .
H2 H 0.546362 0.354106 0.571324 0.041 Uiso 1 1 calc R U . . .
C3 C 0.6397(4) 0.3986(5) 0.5052(5) 0.0267(14) Uani 1 1 d . . . . .
C11 C 0.6502(4) 0.3067(5) 0.4381(5) 0.0283(15) Uani 1 1 d . . . . .
H11A H 0.600820 0.278125 0.415647 0.034 Uiso 1 1 calc R U . . .
H11B H 0.673131 0.327681 0.373754 0.034 Uiso 1 1 calc R U . . .
N3 N 0.6975(3) 0.2263(5) 0.4926(5) 0.0294(13) Uani 1 1 d . . . . .
C12 C 0.7074(6) 0.1461(7) 0.4115(7) 0.052(2) Uani 1 1 d . . . . .
H12A H 0.732529 0.174703 0.353249 0.078 Uiso 1 1 calc R U . . .
H12B H 0.658735 0.120226 0.384554 0.078 Uiso 1 1 calc R U . . .
H12C H 0.737447 0.091420 0.444045 0.078 Uiso 1 1 calc R U . . .
C13 C 0.6595(4) 0.1808(7) 0.5816(6) 0.0406(19) Uani 1 1 d . . . . .
H13A H 0.688283 0.123144 0.610083 0.061 Uiso 1 1 calc R U . . .
H13B H 0.609619 0.158734 0.555505 0.061 Uiso 1 1 calc R U . . .
H13C H 0.655979 0.230843 0.637279 0.061 Uiso 1 1 calc R U . . .
C14 C 0.7717(4) 0.2651(7) 0.5337(7) 0.044(2) Uani 1 1 d . . . . .
H14A H 0.800506 0.211025 0.569710 0.067 Uiso 1 1 calc R U . . .
H14B H 0.765382 0.319830 0.583504 0.067 Uiso 1 1 calc R U . . .
H14C H 0.798113 0.290071 0.474936 0.067 Uiso 1 1 calc R U . . .
C15 C 0.8862(4) 0.7611(5) 0.4329(5) 0.0268(14) Uani 1 1 d . . . . .
H15A H 0.886724 0.832435 0.411463 0.032 Uiso 1 1 calc R U . . .
H15B H 0.873312 0.720816 0.368652 0.032 Uiso 1 1 calc R U . . .
C4 C 0.6866(4) 0.4784(5) 0.5036(5) 0.0244(14) Uani 1 1 d . . . . .
H4 H 0.727073 0.475594 0.460863 0.029 Uiso 1 1 calc R U . . .
C5 C 0.6764(4) 0.5633(5) 0.5628(5) 0.0227(13) Uani 1 1 d . . . . .
C6 C 0.7248(3) 0.6501(5) 0.5645(5) 0.0233(14) Uani 1 1 d . . . . .
C7 C 0.7836(4) 0.6607(5) 0.5008(5) 0.0228(13) Uani 1 1 d . . . . .
H7 H 0.794056 0.608545 0.453487 0.027 Uiso 1 1 calc R U . . .
C8 C 0.8270(4) 0.7471(5) 0.5061(5) 0.0247(14) Uani 1 1 d . . . . .
C16 C 1.0140(5) 0.7445(8) 0.3905(7) 0.055(3) Uani 1 1 d . . . . .
H16A H 1.063783 0.720443 0.414392 0.083 Uiso 1 1 calc R U . . .
H16B H 1.016439 0.815518 0.371351 0.083 Uiso 1 1 calc R U . . .
H16C H 0.994343 0.705662 0.329008 0.083 Uiso 1 1 calc R U . . .
N4 N 0.9637(3) 0.7322(4) 0.4780(4) 0.0254(12) Uani 1 1 d . . . . .
C17 C 0.9903(5) 0.7976(8) 0.5670(7) 0.052(2) Uani 1 1 d . . . . .
H17A H 0.959686 0.787103 0.625862 0.078 Uiso 1 1 calc R U . . .
H17B H 0.986924 0.867872 0.544669 0.078 Uiso 1 1 calc R U . . .
H17C H 1.042110 0.781228 0.589629 0.078 Uiso 1 1 calc R U . . .
C18 C 0.9655(4) 0.6260(6) 0.5109(7) 0.0402(19) Uani 1 1 d . . . . .
H18A H 1.016818 0.606405 0.532550 0.060 Uiso 1 1 calc R U . . .
H18B H 0.945939 0.583951 0.451814 0.060 Uiso 1 1 calc R U . . .
H18C H 0.935065 0.617215 0.570250 0.060 Uiso 1 1 calc R U . . .
C21 C 0.6122(4) 0.8237(8) 0.7737(6) 0.042(2) Uani 1 1 d . . . . .
C9 C 0.8096(4) 0.8196(6) 0.5772(6) 0.0335(16) Uani 1 1 d . . . . .
H9 H 0.838251 0.879257 0.584279 0.040 Uiso 1 1 calc R U . . .
C10 C 0.7506(4) 0.8059(6) 0.6386(6) 0.0343(17) Uani 1 1 d . . . . .
H10 H 0.739381 0.857214 0.686353 0.041 Uiso 1 1 calc R U . . .
N2 N 0.7092(3) 0.7232(5) 0.6327(5) 0.0330(14) Uani 1 1 d . . . . .
O1 O 0.6899(3) 0.6075(5) 0.8955(5) 0.0504(16) Uani 1 1 d . . . . .
C22 C 0.5224(6) 0.6763(7) 0.7543(6) 0.050(2) Uani 1 1 d . . . . .
O2 O 0.6074(3) 0.8967(5) 0.8139(5) 0.0501(16) Uani 1 1 d . . . . .
C23 C 0.6620(4) 0.6437(7) 0.8237(7) 0.0397(19) Uani 1 1 d . . . . .
O3 O 0.4692(3) 0.6621(5) 0.7776(4) 0.0486(16) Uani 1 1 d . . . . .
P1 P 0.86667(12) 0.02349(15) 0.25515(15) 0.0341(4) Uani 1 1 d . . . . .
F11 F 0.8672(4) -0.0939(4) 0.2359(4) 0.077(2) Uani 1 1 d . . . . .
F12 F 0.8667(3) 0.0391(4) 0.1301(3) 0.0453(12) Uani 1 1 d . . . . .
F13 F 0.8663(3) 0.1404(3) 0.2735(4) 0.0463(12) Uani 1 1 d . . . . .
F14 F 0.8652(4) 0.0066(4) 0.3783(3) 0.0683(18) Uani 1 1 d . . . . .
F15 F 0.7782(3) 0.0252(5) 0.2400(4) 0.0557(14) Uani 1 1 d . . . . .
F16 F 0.9537(3) 0.0247(6) 0.2663(5) 0.087(2) Uani 1 1 d . . . . .
P2 P 0.84003(11) 0.44114(14) 0.27224(14) 0.0289(4) Uani 1 1 d . . . . .
F21 F 0.7960(3) 0.3379(4) 0.2733(4) 0.0516(13) Uani 1 1 d . . . . .
F22 F 0.7632(3) 0.4965(4) 0.2808(4) 0.0517(13) Uani 1 1 d . . . . .
F23 F 0.8803(3) 0.5465(4) 0.2736(4) 0.0472(12) Uani 1 1 d . . . . .
F24 F 0.9156(3) 0.3833(4) 0.2655(4) 0.0535(13) Uani 1 1 d . . . . .
F25 F 0.8289(3) 0.4446(4) 0.1466(3) 0.0510(13) Uani 1 1 d . . . . .
F26 F 0.8532(3) 0.4375(4) 0.3982(3) 0.0397(10) Uani 1 1 d . . . . .
O1S O 0.5444(13) 0.0223(17) 0.3902(18) 0.070(6) Uani 0.3333 1 d . . P . .


_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
Br1 Mn1 2.5340(16) . ?
Mn1 C23 1.829(9) . ?
Mn1 C21 1.835(10) . ?
Mn1 C22 1.844(11) . ?
Mn1 N1 2.053(6) . ?
Mn1 N2 2.054(6) . ?
N1 C1 1.330(10) . ?
N1 C5 1.353(8) . ?
C1 C2 1.370(11) . ?
C1 H1 0.9500 . ?
C2 C3 1.390(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.362(10) . ?
C3 C11 1.515(10) . ?
C11 N3 1.505(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N3 C14 1.491(9) . ?
N3 C13 1.503(9) . ?
N3 C12 1.508(10) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C8 1.491(10) . ?
C15 N4 1.517(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C4 C5 1.383(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.451(9) . ?
C6 N2 1.352(8) . ?
C6 C7 1.400(9) . ?
C7 C8 1.392(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.379(10) . ?
C16 N4 1.506(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N4 C18 1.478(9) . ?
N4 C17 1.478(9) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C21 O2 1.108(11) . ?
C9 C10 1.388(10) . ?
C9 H9 0.9500 . ?
C10 N2 1.331(10) . ?
C10 H10 0.9500 . ?
O1 C23 1.114(10) . ?
C22 O3 1.048(11) . ?
P1 F16 1.569(6) . ?
P1 F13 1.577(5) . ?
P1 F11 1.586(5) . ?
P1 F14 1.587(5) . ?
P1 F15 1.595(5) . ?
P1 F12 1.606(5) . ?
P2 F24 1.578(5) . ?
P2 F23 1.583(5) . ?
P2 F22 1.586(5) . ?
P2 F21 1.592(5) . ?
P2 F25 1.595(4) . ?
P2 F26 1.601(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C23 Mn1 C21 91.4(4) . . ?
C23 Mn1 C22 91.8(4) . . ?
C21 Mn1 C22 87.7(4) . . ?
C23 Mn1 N1 91.3(3) . . ?
C21 Mn1 N1 176.0(3) . . ?
C22 Mn1 N1 95.2(3) . . ?
C23 Mn1 N2 94.3(3) . . ?
C21 Mn1 N2 98.0(3) . . ?
C22 Mn1 N2 171.5(3) . . ?
N1 Mn1 N2 78.8(2) . . ?
C23 Mn1 Br1 179.0(3) . . ?
C21 Mn1 Br1 87.6(3) . . ?
C22 Mn1 Br1 88.6(3) . . ?
N1 Mn1 Br1 89.63(19) . . ?
N2 Mn1 Br1 85.39(18) . . ?
C1 N1 C5 117.9(6) . . ?
C1 N1 Mn1 126.9(5) . . ?
C5 N1 Mn1 115.2(5) . . ?
N1 C1 C2 123.0(7) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 120.0(7) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 116.8(7) . . ?
C4 C3 C11 121.0(6) . . ?
C2 C3 C11 122.2(7) . . ?
N3 C11 C3 114.3(6) . . ?
N3 C11 H11A 108.7 . . ?
C3 C11 H11A 108.7 . . ?
N3 C11 H11B 108.7 . . ?
C3 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C14 N3 C13 109.4(6) . . ?
C14 N3 C11 111.9(6) . . ?
C13 N3 C11 110.9(5) . . ?
C14 N3 C12 109.3(6) . . ?
C13 N3 C12 108.6(6) . . ?
C11 N3 C12 106.7(6) . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C14 H14A 109.5 . . ?
N3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C8 C15 N4 114.9(5) . . ?
C8 C15 H15A 108.5 . . ?
N4 C15 H15A 108.5 . . ?
C8 C15 H15B 108.5 . . ?
N4 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C3 C4 C5 121.3(6) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
N1 C5 C4 121.1(6) . . ?
N1 C5 C6 115.3(6) . . ?
C4 C5 C6 123.6(6) . . ?
N2 C6 C7 120.7(6) . . ?
N2 C6 C5 115.2(6) . . ?
C7 C6 C5 124.1(6) . . ?
C8 C7 C6 120.6(6) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C9 C8 C7 116.9(7) . . ?
C9 C8 C15 122.6(7) . . ?
C7 C8 C15 120.4(6) . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 N4 C17 110.5(6) . . ?
C18 N4 C16 108.3(7) . . ?
C17 N4 C16 109.0(7) . . ?
C18 N4 C15 110.4(5) . . ?
C17 N4 C15 111.7(6) . . ?
C16 N4 C15 106.9(6) . . ?
N4 C17 H17A 109.5 . . ?
N4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O2 C21 Mn1 176.5(7) . . ?
C8 C9 C10 120.5(7) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
N2 C10 C9 122.3(7) . . ?
N2 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 N2 C6 119.1(6) . . ?
C10 N2 Mn1 125.4(5) . . ?
C6 N2 Mn1 115.2(5) . . ?
O3 C22 Mn1 177.4(8) . . ?
O1 C23 Mn1 178.6(8) . . ?
F16 P1 F13 89.6(3) . . ?
F16 P1 F11 90.2(4) . . ?
F13 P1 F11 179.6(3) . . ?
F16 P1 F14 90.9(4) . . ?
F13 P1 F14 89.7(3) . . ?
F11 P1 F14 90.7(3) . . ?
F16 P1 F15 177.8(4) . . ?
F13 P1 F15 89.3(3) . . ?
F11 P1 F15 90.9(4) . . ?
F14 P1 F15 91.1(3) . . ?
F16 P1 F12 90.1(3) . . ?
F13 P1 F12 91.1(3) . . ?
F11 P1 F12 88.5(3) . . ?
F14 P1 F12 178.8(4) . . ?
F15 P1 F12 88.0(3) . . ?
F24 P2 F23 92.0(3) . . ?
F24 P2 F22 178.3(3) . . ?
F23 P2 F22 89.5(3) . . ?
F24 P2 F21 90.8(3) . . ?
F23 P2 F21 177.1(3) . . ?
F22 P2 F21 87.7(3) . . ?
F24 P2 F25 89.7(3) . . ?
F23 P2 F25 90.2(3) . . ?
F22 P2 F25 91.2(3) . . ?
F21 P2 F25 90.8(3) . . ?
F24 P2 F26 89.2(3) . . ?
F23 P2 F26 89.3(3) . . ?
F22 P2 F26 90.0(3) . . ?
F21 P2 F26 89.8(3) . . ?
F25 P2 F26 178.7(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 -0.8(12) . . . . ?
Mn1 N1 C1 C2 -178.6(6) . . . . ?
N1 C1 C2 C3 0.6(13) . . . . ?
C1 C2 C3 C4 -0.6(11) . . . . ?
C1 C2 C3 C11 -178.2(7) . . . . ?
C4 C3 C11 N3 91.7(8) . . . . ?
C2 C3 C11 N3 -90.7(8) . . . . ?
C3 C11 N3 C14 -55.5(8) . . . . ?
C3 C11 N3 C13 66.9(8) . . . . ?
C3 C11 N3 C12 -174.9(6) . . . . ?
C2 C3 C4 C5 0.8(10) . . . . ?
C11 C3 C4 C5 178.5(6) . . . . ?
C1 N1 C5 C4 1.1(10) . . . . ?
Mn1 N1 C5 C4 179.1(5) . . . . ?
C1 N1 C5 C6 -179.6(6) . . . . ?
Mn1 N1 C5 C6 -1.5(8) . . . . ?
C3 C4 C5 N1 -1.1(10) . . . . ?
C3 C4 C5 C6 179.6(6) . . . . ?
N1 C5 C6 N2 5.1(9) . . . . ?
C4 C5 C6 N2 -175.6(6) . . . . ?
N1 C5 C6 C7 -174.3(6) . . . . ?
C4 C5 C6 C7 5.1(11) . . . . ?
N2 C6 C7 C8 -0.2(10) . . . . ?
C5 C6 C7 C8 179.1(6) . . . . ?
C6 C7 C8 C9 0.7(10) . . . . ?
C6 C7 C8 C15 -175.8(6) . . . . ?
N4 C15 C8 C9 86.9(8) . . . . ?
N4 C15 C8 C7 -96.8(7) . . . . ?
C8 C15 N4 C18 58.4(8) . . . . ?
C8 C15 N4 C17 -65.0(8) . . . . ?
C8 C15 N4 C16 176.0(7) . . . . ?
C7 C8 C9 C10 -1.0(11) . . . . ?
C15 C8 C9 C10 175.4(7) . . . . ?
C8 C9 C10 N2 0.7(12) . . . . ?
C9 C10 N2 C6 -0.2(11) . . . . ?
C9 C10 N2 Mn1 -172.7(6) . . . . ?
C7 C6 N2 C10 0.0(10) . . . . ?
C5 C6 N2 C10 -179.4(6) . . . . ?
C7 C6 N2 Mn1 173.2(5) . . . . ?
C5 C6 N2 Mn1 -6.2(8) . . . . ?

_refine_diff_density_max         0.666
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.127



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl Ether/acetonitrile'
_chemical_properties_physical    Light-sensitive
####################################################################### 
# 
# 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_P17338
_database_code_depnum_ccdc_archive 'CCDC 2494315'
loop_
_audit_author_name
_audit_author_address
'Michael K. Takase'
;California Institute of Technology
United States of America
;
_audit_update_record             
;
2025-10-15 deposited with the CCDC.	2026-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23H31N5O3Re2+ 3(F6P-) 0.5(H3C2N) 0.5(H10C2O)'
_chemical_formula_sum            'C28 H40.50 F18 N6.50 O3.50 P3 Re'
_chemical_formula_weight         1145.28

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                   13.0356(6)
_cell_length_b                   13.2377(6)
_cell_length_c                   14.7412(7)
_cell_angle_alpha                113.8926(17)
_cell_angle_beta                 96.814(2)
_cell_angle_gamma                111.3674(18)
_cell_volume                     2057.32(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9959
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      32.05

_exptl_crystal_description       Block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.193
_shelx_estimated_absorpt_T_min   0.401
_shelx_estimated_absorpt_T_max   0.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6088
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            60104
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.243
_diffrn_reflns_theta_max         36.384
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             19968
_reflns_number_gt                15842
_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       'APEX3 v2017.3-0 (Bruker-AXS, 2017)'
_computing_cell_refinement       'SAINT v8.38A (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT v8.38A (Bruker-AXS, 2013)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0233P)²+1.2926P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         19968
_refine_ls_number_parameters     773
_refine_ls_number_restraints     1498
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0717
_refine_ls_wR_factor_gt          0.0665
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      2.507
_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 0.59114(2) 0.41224(2) 0.16091(2) 0.01663(2) Uani 1 1 d D . . . .
N1 N 0.57656(16) 0.28374(16) 0.22034(14) 0.0163(3) Uani 1 1 d . . . . .
C1 C 0.54044(19) 0.16158(19) 0.16122(17) 0.0189(4) Uani 1 1 d . . . . .
H1 H 0.517099 0.126778 0.087385 0.023 Uiso 1 1 calc R U . . .
C2 C 0.53579(19) 0.08417(19) 0.20333(17) 0.0191(4) Uani 1 1 d . . . . .
H2 H 0.507849 -0.002207 0.158878 0.023 Uiso 1 1 calc R U . . .
C3 C 0.57205(18) 0.13357(19) 0.31032(17) 0.0172(4) Uani 1 1 d . . . . .
C31 C 0.57168(18) 0.05676(19) 0.36281(18) 0.0182(4) Uani 1 1 d . . . . .
H31A H 0.504622 -0.026471 0.320121 0.022 Uiso 1 1 calc R U . . .
H31B H 0.560706 0.095791 0.431626 0.022 Uiso 1 1 calc R U . . .
N3 N 0.68125(16) 0.04162(16) 0.37893(15) 0.0185(3) Uani 1 1 d . . . . .
C32 C 0.6820(2) -0.0515(2) 0.2789(2) 0.0289(5) Uani 1 1 d . . . . .
H32A H 0.751916 -0.062249 0.291403 0.043 Uiso 1 1 calc R U . . .
H32B H 0.681430 -0.022377 0.227497 0.043 Uiso 1 1 calc R U . . .
H32C H 0.613138 -0.131035 0.252164 0.043 Uiso 1 1 calc R U . . .
C33 C 0.6819(2) -0.0034(2) 0.4573(2) 0.0281(5) Uani 1 1 d . . . . .
H33A H 0.612198 -0.082055 0.430984 0.042 Uiso 1 1 calc R U . . .
H33B H 0.682877 0.058315 0.523361 0.042 Uiso 1 1 calc R U . . .
H33C H 0.750974 -0.015725 0.468753 0.042 Uiso 1 1 calc R U . . .
C34 C 0.7885(2) 0.1620(2) 0.4205(2) 0.0269(5) Uani 1 1 d . . . . .
H34A H 0.857195 0.149957 0.435409 0.040 Uiso 1 1 calc R U . . .
H34B H 0.787321 0.224402 0.484794 0.040 Uiso 1 1 calc R U . . .
H34C H 0.791138 0.190190 0.368348 0.040 Uiso 1 1 calc R U . . .
C4 C 0.60719(19) 0.25970(19) 0.37197(17) 0.0178(4) Uani 1 1 d . . . . .
H4 H 0.631136 0.296142 0.445937 0.021 Uiso 1 1 calc R U . . .
C5 C 0.60724(18) 0.33171(18) 0.32572(16) 0.0158(4) Uani 1 1 d . . . . .
N2 N 0.63295(17) 0.52165(17) 0.32895(14) 0.0203(4) Uani 1 1 d . . . . .
C6 C 0.63742(19) 0.46420(19) 0.38633(16) 0.0169(4) Uani 1 1 d . . . . .
C7 C 0.66565(19) 0.52612(19) 0.49448(17) 0.0187(4) Uani 1 1 d . . . . .
H7 H 0.666826 0.483271 0.532696 0.022 Uiso 1 1 calc R U . . .
C8 C 0.6922(2) 0.6511(2) 0.54661(17) 0.0195(4) Uani 1 1 d . . . . .
C41 C 0.72245(19) 0.7222(2) 0.66344(17) 0.0198(4) Uani 1 1 d . . . . .
H41A H 0.675587 0.666260 0.687443 0.024 Uiso 1 1 calc R U . . .
H41B H 0.700663 0.790509 0.681424 0.024 Uiso 1 1 calc R U . . .
N4 N 0.84967(16) 0.77641(17) 0.72217(14) 0.0193(4) Uani 1 1 d . . . . .
C42 C 0.8790(2) 0.6759(2) 0.7203(2) 0.0302(6) Uani 1 1 d . . . . .
H42A H 0.865572 0.616833 0.647927 0.045 Uiso 1 1 calc R U . . .
H42B H 0.829944 0.632646 0.751279 0.045 Uiso 1 1 calc R U . . .
H42C H 0.960725 0.712799 0.760475 0.045 Uiso 1 1 calc R U . . .
C43 C 0.8710(2) 0.8655(2) 0.83341(18) 0.0295(5) Uani 1 1 d . . . . .
H43A H 0.819696 0.822313 0.863138 0.044 Uiso 1 1 calc R U . . .
H43B H 0.855280 0.933519 0.836153 0.044 Uiso 1 1 calc R U . . .
H43C H 0.951974 0.899079 0.873728 0.044 Uiso 1 1 calc R U . . .
C44 C 0.9260(2) 0.8446(3) 0.6774(2) 0.0354(6) Uani 1 1 d . . . . .
H44A H 1.006657 0.887478 0.722038 0.053 Uiso 1 1 calc R U . . .
H44B H 0.902347 0.905474 0.673491 0.053 Uiso 1 1 calc R U . . .
H44C H 0.918975 0.785741 0.607107 0.053 Uiso 1 1 calc R U . . .
C9 C 0.6858(3) 0.7083(2) 0.48729(19) 0.0307(6) Uani 1 1 d . . . . .
H9 H 0.701615 0.793044 0.520154 0.037 Uiso 1 1 calc R U . . .
C10 C 0.6564(3) 0.6417(2) 0.38009(19) 0.0317(6) Uani 1 1 d . . . . .
H10 H 0.652578 0.682539 0.340548 0.038 Uiso 1 1 calc R U . . .
C11 C 0.6100(2) 0.5420(2) 0.12581(18) 0.0238(5) Uani 1 1 d . . . . .
O1 O 0.61869(18) 0.61930(17) 0.10522(15) 0.0341(4) Uani 1 1 d . . . . .
C12 C 0.5634(2) 0.3027(2) 0.01660(18) 0.0223(4) Uani 1 1 d . . . . .
O2 O 0.54927(17) 0.23779(16) -0.06903(13) 0.0294(4) Uani 1 1 d . . . . .
C13 C 0.4276(2) 0.3637(2) 0.12790(18) 0.0250(5) Uani 1 1 d . . . . .
O3 O 0.33052(17) 0.33199(19) 0.10594(16) 0.0362(4) Uani 1 1 d . . . . .
N5 N 0.7719(8) 0.464(2) 0.2072(12) 0.020(2) Uani 0.52(3) 1 d D U P A 1
C51 C 0.8678(7) 0.4941(13) 0.2255(9) 0.0281(19) Uani 0.52(3) 1 d D U P A 1
C52 C 0.9913(7) 0.5322(16) 0.2516(11) 0.046(2) Uani 0.52(3) 1 d D U P A 1
H52A H 1.008361 0.482268 0.191029 0.070 Uiso 0.52(3) 1 calc R U P A 1
H52B H 1.015938 0.520131 0.310299 0.070 Uiso 0.52(3) 1 calc R U P A 1
H52C H 1.033159 0.620018 0.271251 0.070 Uiso 0.52(3) 1 calc R U P A 1
N5B N 0.7703(9) 0.451(2) 0.1855(14) 0.023(2) Uani 0.48(3) 1 d D U P A 2
C51B C 0.8621(8) 0.4640(12) 0.1928(14) 0.034(2) Uani 0.48(3) 1 d D U P A 2
C52B C 0.9812(7) 0.4841(13) 0.2002(17) 0.049(4) Uani 0.48(3) 1 d D U P A 2
H52D H 1.013819 0.533863 0.167015 0.074 Uiso 0.48(3) 1 calc R U P A 2
H52E H 0.982063 0.403968 0.164766 0.074 Uiso 0.48(3) 1 calc R U P A 2
H52F H 1.027755 0.528097 0.273902 0.074 Uiso 0.48(3) 1 calc R U P A 2
P1 P 0.63047(6) 0.33531(6) 0.68212(5) 0.02573(13) Uani 1 1 d D . . B 2
F11 F 0.52993(13) 0.25353(14) 0.57048(12) 0.0309(3) Uani 1 1 d D . . B 2
F12 F 0.63353(17) 0.21122(15) 0.67008(15) 0.0470(5) Uani 1 1 d D . . B 2
F13 F 0.73009(16) 0.41566(16) 0.79052(13) 0.0455(4) Uani 1 1 d D . . B 2
F14 F 0.62282(17) 0.45600(15) 0.68909(14) 0.0423(4) Uani 1 1 d D . . B 2
F15 F 0.53353(17) 0.31456(18) 0.73817(14) 0.0475(5) Uani 1 1 d D . . B 2
F16 F 0.72441(14) 0.35492(16) 0.62280(13) 0.0382(4) Uani 1 1 d D . . B 2
P2 P 0.77628(6) 0.06892(7) 0.05346(5) 0.03204(15) Uani 1 1 d . . . C 2
F21 F 0.83512(16) -0.01858(18) 0.05379(15) 0.0468(4) Uani 1 1 d . . . C 2
F22 F 0.65997(14) -0.02473(16) 0.05792(12) 0.0392(4) Uani 1 1 d . . . C 2
F23 F 0.71779(19) 0.1554(2) 0.05189(17) 0.0550(5) Uani 1 1 d . . . C 2
F24 F 0.89345(15) 0.16184(19) 0.04894(15) 0.0492(5) Uani 1 1 d . . . C 2
F25 F 0.82332(16) 0.14287(17) 0.17778(13) 0.0491(5) Uani 1 1 d . . . C 2
F26 F 0.72976(16) -0.0056(2) -0.07104(13) 0.0480(5) Uani 1 1 d . . . C 2
P3 P 0.9857(3) 0.5041(3) 0.4859(2) 0.0336(6) Uani 0.5 1 d D U P D -1
F31 F 0.9119(8) 0.4015(8) 0.3678(5) 0.0516(19) Uani 0.5 1 d D U P D -1
F32 F 0.9477(7) 0.6006(7) 0.4745(6) 0.0584(19) Uani 0.5 1 d D U P D -1
F35 F 0.8747(6) 0.4532(8) 0.5205(6) 0.0349(12) Uani 0.5 1 d D U P D -1
F33 F 1.0601(7) 0.6043(7) 0.6052(5) 0.053(2) Uani 0.5 1 d D U P D -1
F34 F 1.0239(6) 0.4087(6) 0.4998(6) 0.0502(15) Uani 0.5 1 d D U P D -1
F36 F 1.0974(6) 0.5534(7) 0.4521(6) 0.063(2) Uani 0.5 1 d D U P D -1
P4 P 0.95095(19) 0.8711(2) 0.4010(2) 0.0317(6) Uani 0.381(3) 1 d D U P E -1
F41 F 0.9446(5) 0.9792(5) 0.3820(6) 0.0521(16) Uani 0.381(3) 1 d D U P E -1
F42 F 0.8726(4) 0.8929(4) 0.4745(4) 0.0417(12) Uani 0.381(3) 1 d D U P E -1
F43 F 0.9529(5) 0.7658(5) 0.4260(4) 0.0533(15) Uani 0.381(3) 1 d D U P E -1
F44 F 1.0315(6) 0.8539(7) 0.3311(6) 0.074(2) Uani 0.381(3) 1 d D U P E -1
F45 F 0.8366(5) 0.7730(6) 0.3043(6) 0.0456(16) Uani 0.381(3) 1 d D U P E -1
F46 F 1.0621(4) 0.9712(5) 0.5017(5) 0.071(2) Uani 0.381(3) 1 d D U P E -1
P4B P 0.9706(6) 0.8711(6) 0.3653(6) 0.0285(16) Uani 0.119(3) 1 d D U P E -2
F41B F 0.9815(18) 0.8836(15) 0.2650(10) 0.080(6) Uani 0.119(3) 1 d D U P E -2
F42B F 0.9011(17) 0.947(2) 0.3846(19) 0.087(7) Uani 0.119(3) 1 d D U P E -2
F43B F 0.9617(17) 0.8679(17) 0.4713(10) 0.076(6) Uani 0.119(3) 1 d D U P E -2
F44B F 1.0454(18) 0.7965(19) 0.3533(19) 0.075(6) Uani 0.119(3) 1 d D U P E -2
F45B F 0.8592(15) 0.7447(15) 0.2991(16) 0.070(7) Uani 0.119(3) 1 d D U P E -2
F46B F 1.0876(9) 0.9927(11) 0.4300(12) 0.049(4) Uani 0.119(3) 1 d D U P E -2
O2S O 0.9382(6) 0.7168(6) 0.1827(5) 0.089(2) Uani 0.5 1 d D . P E 2
C21S C 0.9117(8) 0.7470(10) 0.0991(7) 0.060(2) Uani 0.5 1 d D . P E 2
H21A H 0.844999 0.766153 0.100390 0.072 Uiso 0.5 1 calc R U P E 2
H21B H 0.979585 0.818021 0.105340 0.072 Uiso 0.5 1 calc R U P E 2
C22S C 0.8835(13) 0.6320(13) 0.0045(9) 0.079(4) Uani 0.5 1 d D . P E 2
H22A H 0.864115 0.641079 -0.057159 0.119 Uiso 0.5 1 calc R U P E 2
H22B H 0.950465 0.614674 0.006123 0.119 Uiso 0.5 1 calc R U P E 2
H22C H 0.817043 0.563256 0.001215 0.119 Uiso 0.5 1 calc R U P E 2
C23S C 0.9491(11) 0.8131(9) 0.2830(8) 0.089(4) Uani 0.5 1 d D . P E 2
H23A H 0.874336 0.816336 0.282468 0.107 Uiso 0.5 1 calc R U P E 2
H23B H 1.008699 0.895179 0.298212 0.107 Uiso 0.5 1 calc R U P E 2
C24S C 0.9844(10) 0.7795(8) 0.3648(8) 0.073(3) Uani 0.5 1 d D . P E 2
H24A H 0.992893 0.842095 0.433951 0.109 Uiso 0.5 1 calc R U P E 2
H24B H 0.924740 0.698147 0.348718 0.109 Uiso 0.5 1 calc R U P E 2
H24C H 1.058449 0.776607 0.364386 0.109 Uiso 0.5 1 calc R U P E 2
N3S N 0.919(3) 0.557(3) 0.0433(19) 0.093(12) Uani 0.253(14) 1 d D U P F -1
C31S C 0.9078(18) 0.641(3) 0.054(2) 0.077(10) Uani 0.253(14) 1 d D U P F -1
C32S C 0.894(3) 0.748(4) 0.061(3) 0.145(17) Uani 0.253(14) 1 d D U P F -1
H32D H 0.931659 0.775117 0.015161 0.218 Uiso 0.253(14) 1 calc R U P F -1
H32E H 0.930711 0.816417 0.133086 0.218 Uiso 0.253(14) 1 calc R U P F -1
H32F H 0.811676 0.725922 0.038730 0.218 Uiso 0.253(14) 1 calc R U P F -1
N3T N 0.9572(18) 0.5053(16) 0.0062(19) 0.088(8) Uani 0.247(14) 1 d D . P E -2
C31T C 0.907(2) 0.560(3) 0.0171(15) 0.053(6) Uani 0.247(14) 1 d D . P E -2
C32T C 0.854(3) 0.642(3) 0.034(3) 0.078(10) Uani 0.247(14) 1 d D . P E -2
H32G H 0.798560 0.615051 -0.032147 0.117 Uiso 0.247(14) 1 calc R U P F -2
H32H H 0.914543 0.726989 0.059092 0.117 Uiso 0.247(14) 1 calc R U P F -2
H32I H 0.814188 0.640965 0.085736 0.117 Uiso 0.247(14) 1 calc R U P F -2
N1S N 0.2853(3) 0.0108(2) 0.3126(2) 0.0456(7) Uani 1 1 d D . . . .
C11S C 0.2525(2) -0.0843(3) 0.2431(2) 0.0300(5) Uani 1 1 d D . . . .
C12S C 0.2120(3) -0.2058(3) 0.1525(2) 0.0443(8) Uani 1 1 d D . . . .
H12A H 0.171519 -0.207884 0.090771 0.066 Uiso 1 1 calc R U . . .
H12B H 0.158698 -0.269713 0.164923 0.066 Uiso 1 1 calc R U . . .
H12C H 0.278408 -0.221419 0.140720 0.066 Uiso 1 1 calc 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 C13 1.922(3) . ?
Re1 C12 1.922(2) . ?
Re1 C11 1.929(2) . ?
Re1 N5 2.133(8) . ?
Re1 N5B 2.151(8) . ?
Re1 N1 2.1699(17) . ?
Re1 N2 2.1746(18) . ?
N1 C1 1.343(3) . ?
N1 C5 1.358(3) . ?
C1 C2 1.385(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.379(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.392(3) . ?
C3 C31 1.506(3) . ?
C31 N3 1.518(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
N3 C32 1.495(3) . ?
N3 C33 1.499(3) . ?
N3 C34 1.501(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C4 C5 1.378(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.474(3) . ?
N2 C10 1.345(3) . ?
N2 C6 1.356(3) . ?
C6 C7 1.390(3) . ?
C7 C8 1.391(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(3) . ?
C8 C41 1.504(3) . ?
C41 N4 1.518(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
N4 C44 1.492(3) . ?
N4 C43 1.498(3) . ?
N4 C42 1.504(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C9 C10 1.379(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 O1 1.152(3) . ?
C12 O2 1.147(3) . ?
C13 O3 1.135(3) . ?
N5 C51 1.125(8) . ?
C51 C52 1.449(8) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
N5B C51B 1.129(9) . ?
C51B C52B 1.459(9) . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?
P1 F13 1.5797(18) . ?
P1 F15 1.5917(18) . ?
P1 F16 1.5932(17) . ?
P1 F12 1.5953(17) . ?
P1 F14 1.5995(16) . ?
P1 F11 1.6153(16) . ?
P2 F25 1.5922(17) . ?
P2 F26 1.5946(17) . ?
P2 F23 1.596(2) . ?
P2 F22 1.5999(18) . ?
P2 F24 1.6038(19) . ?
P2 F21 1.607(2) . ?
P3 F32 1.587(5) . ?
P3 F34 1.590(5) . ?
P3 F31 1.593(6) . ?
P3 F36 1.593(7) . ?
P3 F35 1.598(7) . ?
P3 F33 1.601(6) . ?
P4 F44 1.567(6) . ?
P4 F43 1.587(5) . ?
P4 F42 1.589(5) . ?
P4 F45 1.589(5) . ?
P4 F41 1.593(5) . ?
P4 F46 1.598(5) . ?
P4B C23S 1.070(12) . ?
P4B C24S 1.287(12) . ?
P4B F42B 1.547(11) . ?
P4B F45B 1.560(11) . ?
P4B F46B 1.565(10) . ?
P4B F41B 1.569(10) . ?
P4B F43B 1.597(10) . ?
P4B F44B 1.600(11) . ?
F41B C23S 1.029(16) . ?
F43B C24S 1.67(2) . ?
F44B C24S 0.80(2) . ?
F44B C23S 1.67(2) . ?
F45B C23S 1.31(2) . ?
F45B C24S 1.59(2) . ?
O2S C23S 1.458(10) . ?
O2S C21S 1.482(11) . ?
C21S C32T 1.18(4) . ?
C21S C22S 1.467(14) . ?
C21S H21A 0.9900 . ?
C21S H21B 0.9900 . ?
C22S C32T 0.62(2) . ?
C22S C31T 1.18(3) . ?
C22S H22A 0.9800 . ?
C22S H22B 0.9800 . ?
C22S H22C 0.9800 . ?
C23S C24S 1.522(13) . ?
C23S H23A 0.9900 . ?
C23S H23B 0.9900 . ?
C24S H24A 0.9800 . ?
C24S H24B 0.9800 . ?
C24S H24C 0.9800 . ?
N3S C31S 1.129(15) . ?
C31S C32S 1.458(15) . ?
C32S H32D 0.9800 . ?
C32S H32E 0.9800 . ?
C32S H32F 0.9800 . ?
N3T C31T 1.113(14) . ?
C31T C32T 1.453(14) . ?
C32T H32G 0.9800 . ?
C32T H32H 0.9800 . ?
C32T H32I 0.9800 . ?
N1S C11S 1.130(4) . ?
C11S C12S 1.457(4) . ?
C12S H12A 0.9800 . ?
C12S H12B 0.9800 . ?
C12S H12C 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
C13 Re1 C12 88.01(10) . . ?
C13 Re1 C11 88.40(10) . . ?
C12 Re1 C11 88.55(9) . . ?
C13 Re1 N5 175.9(6) . . ?
C12 Re1 N5 94.9(4) . . ?
C11 Re1 N5 94.6(7) . . ?
C13 Re1 N5B 174.8(6) . . ?
C12 Re1 N5B 87.2(5) . . ?
C11 Re1 N5B 93.5(8) . . ?
C13 Re1 N1 92.62(9) . . ?
C12 Re1 N1 98.48(8) . . ?
C11 Re1 N1 172.92(8) . . ?
N5 Re1 N1 84.0(7) . . ?
N5B Re1 N1 86.0(8) . . ?
C13 Re1 N2 96.28(9) . . ?
C12 Re1 N2 172.18(8) . . ?
C11 Re1 N2 98.07(8) . . ?
N5 Re1 N2 80.5(4) . . ?
N5B Re1 N2 88.3(5) . . ?
N1 Re1 N2 74.85(7) . . ?
C1 N1 C5 117.96(18) . . ?
C1 N1 Re1 125.11(14) . . ?
C5 N1 Re1 116.93(13) . . ?
N1 C1 C2 122.8(2) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 119.4(2) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 117.99(19) . . ?
C2 C3 C31 123.03(19) . . ?
C4 C3 C31 118.95(19) . . ?
C3 C31 N3 114.27(17) . . ?
C3 C31 H31A 108.7 . . ?
N3 C31 H31A 108.7 . . ?
C3 C31 H31B 108.7 . . ?
N3 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
C32 N3 C33 109.34(18) . . ?
C32 N3 C34 109.0(2) . . ?
C33 N3 C34 108.70(18) . . ?
C32 N3 C31 110.69(17) . . ?
C33 N3 C31 107.16(18) . . ?
C34 N3 C31 111.90(17) . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N3 C34 H34A 109.5 . . ?
N3 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N3 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C5 C4 C3 120.0(2) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N1 C5 C4 121.74(19) . . ?
N1 C5 C6 115.57(17) . . ?
C4 C5 C6 122.68(19) . . ?
C10 N2 C6 117.80(19) . . ?
C10 N2 Re1 125.15(15) . . ?
C6 N2 Re1 117.04(14) . . ?
N2 C6 C7 121.81(19) . . ?
N2 C6 C5 115.31(18) . . ?
C7 C6 C5 122.86(18) . . ?
C6 C7 C8 119.8(2) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C9 C8 C7 117.9(2) . . ?
C9 C8 C41 120.09(19) . . ?
C7 C8 C41 121.9(2) . . ?
C8 C41 N4 114.28(18) . . ?
C8 C41 H41A 108.7 . . ?
N4 C41 H41A 108.7 . . ?
C8 C41 H41B 108.7 . . ?
N4 C41 H41B 108.7 . . ?
H41A C41 H41B 107.6 . . ?
C44 N4 C43 108.7(2) . . ?
C44 N4 C42 109.8(2) . . ?
C43 N4 C42 108.50(18) . . ?
C44 N4 C41 111.33(18) . . ?
C43 N4 C41 107.95(18) . . ?
C42 N4 C41 110.52(17) . . ?
N4 C42 H42A 109.5 . . ?
N4 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N4 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C43 H43A 109.5 . . ?
N4 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N4 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N4 C44 H44A 109.5 . . ?
N4 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N4 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C10 C9 C8 119.6(2) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
N2 C10 C9 123.1(2) . . ?
N2 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
O1 C11 Re1 178.3(2) . . ?
O2 C12 Re1 178.5(2) . . ?
O3 C13 Re1 178.0(2) . . ?
C51 N5 Re1 174.5(18) . . ?
N5 C51 C52 178.4(16) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51B N5B Re1 175.6(16) . . ?
N5B C51B C52B 177.7(19) . . ?
C51B C52B H52D 109.5 . . ?
C51B C52B H52E 109.5 . . ?
H52D C52B H52E 109.5 . . ?
C51B C52B H52F 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
F13 P1 F15 91.35(11) . . ?
F13 P1 F16 90.39(10) . . ?
F15 P1 F16 178.16(10) . . ?
F13 P1 F12 91.32(10) . . ?
F15 P1 F12 89.97(11) . . ?
F16 P1 F12 90.60(11) . . ?
F13 P1 F14 91.33(10) . . ?
F15 P1 F14 90.01(10) . . ?
F16 P1 F14 89.34(10) . . ?
F12 P1 F14 177.36(11) . . ?
F13 P1 F11 179.21(11) . . ?
F15 P1 F11 89.44(10) . . ?
F16 P1 F11 88.82(9) . . ?
F12 P1 F11 88.73(9) . . ?
F14 P1 F11 88.62(9) . . ?
F25 P2 F26 179.61(12) . . ?
F25 P2 F23 91.04(12) . . ?
F26 P2 F23 89.34(11) . . ?
F25 P2 F22 89.69(9) . . ?
F26 P2 F22 90.41(10) . . ?
F23 P2 F22 90.39(11) . . ?
F25 P2 F24 90.33(10) . . ?
F26 P2 F24 89.56(11) . . ?
F23 P2 F24 90.20(11) . . ?
F22 P2 F24 179.41(11) . . ?
F25 P2 F21 89.53(11) . . ?
F26 P2 F21 90.09(11) . . ?
F23 P2 F21 179.40(11) . . ?
F22 P2 F21 89.82(10) . . ?
F24 P2 F21 89.59(11) . . ?
F32 P3 F34 178.8(6) . . ?
F32 P3 F31 91.7(4) . . ?
F34 P3 F31 89.3(4) . . ?
F32 P3 F36 91.5(4) . . ?
F34 P3 F36 89.2(4) . . ?
F31 P3 F36 90.9(5) . . ?
F32 P3 F35 89.7(4) . . ?
F34 P3 F35 89.7(4) . . ?
F31 P3 F35 89.3(5) . . ?
F36 P3 F35 178.8(4) . . ?
F32 P3 F33 89.8(4) . . ?
F34 P3 F33 89.2(4) . . ?
F31 P3 F33 178.4(6) . . ?
F36 P3 F33 89.5(5) . . ?
F35 P3 F33 90.3(5) . . ?
F44 P4 F43 92.1(4) . . ?
F44 P4 F42 178.1(4) . . ?
F43 P4 F42 88.7(3) . . ?
F44 P4 F45 92.4(4) . . ?
F43 P4 F45 91.0(4) . . ?
F42 P4 F45 89.3(4) . . ?
F44 P4 F41 91.8(4) . . ?
F43 P4 F41 176.0(4) . . ?
F42 P4 F41 87.3(3) . . ?
F45 P4 F41 89.6(4) . . ?
F44 P4 F46 90.3(4) . . ?
F43 P4 F46 89.3(3) . . ?
F42 P4 F46 88.0(3) . . ?
F45 P4 F46 177.2(4) . . ?
F41 P4 F46 90.0(4) . . ?
C23S P4B C24S 79.8(8) . . ?
C23S P4B F42B 109.5(12) . . ?
C24S P4B F42B 149.1(12) . . ?
C23S P4B F45B 56.1(12) . . ?
C24S P4B F45B 67.2(11) . . ?
F42B P4B F45B 93.0(11) . . ?
C23S P4B F46B 122.1(11) . . ?
C24S P4B F46B 109.2(8) . . ?
F42B P4B F46B 91.1(10) . . ?
F45B P4B F46B 175.9(11) . . ?
C23S P4B F41B 40.7(8) . . ?
C24S P4B F41B 113.6(10) . . ?
F42B P4B F41B 89.2(10) . . ?
F45B P4B F41B 91.0(10) . . ?
F46B P4B F41B 88.9(8) . . ?
C23S P4B F43B 143.0(10) . . ?
C24S P4B F43B 69.9(9) . . ?
F42B P4B F43B 88.1(11) . . ?
F45B P4B F43B 91.8(10) . . ?
F46B P4B F43B 88.5(8) . . ?
F41B P4B F43B 176.2(10) . . ?
C23S P4B F44B 74.3(11) . . ?
C24S P4B F44B 29.8(9) . . ?
F42B P4B F44B 176.2(12) . . ?
F45B P4B F44B 88.8(11) . . ?
F46B P4B F44B 87.1(9) . . ?
F41B P4B F44B 94.1(11) . . ?
F43B P4B F44B 88.5(10) . . ?
C23S F41B P4B 42.6(7) . . ?
P4B F43B C24S 46.3(6) . . ?
C24S F44B P4B 52.9(11) . . ?
C24S F44B C23S 65.6(16) . . ?
P4B F44B C23S 38.2(5) . . ?
C23S F45B P4B 42.7(6) . . ?
C23S F45B C24S 62.4(9) . . ?
P4B F45B C24S 48.2(6) . . ?
C23S O2S C21S 110.1(8) . . ?
C32T C21S C22S 23.9(14) . . ?
C32T C21S O2S 95(2) . . ?
C22S C21S O2S 102.0(10) . . ?
C32T C21S H21A 93.8 . . ?
C22S C21S H21A 111.4 . . ?
O2S C21S H21A 111.4 . . ?
C32T C21S H21B 134.5 . . ?
C22S C21S H21B 111.4 . . ?
O2S C21S H21B 111.4 . . ?
H21A C21S H21B 109.2 . . ?
C32T C22S C31T 103(4) . . ?
C32T C22S C21S 51(4) . . ?
C31T C22S C21S 116.1(14) . . ?
C32T C22S H22A 114.4 . . ?
C31T C22S H22A 132.8 . . ?
C21S C22S H22A 109.5 . . ?
C32T C22S H22B 135.9 . . ?
C31T C22S H22B 44.0 . . ?
C21S C22S H22B 109.5 . . ?
H22A C22S H22B 109.5 . . ?
C32T C22S H22C 59.7 . . ?
C31T C22S H22C 66.4 . . ?
C21S C22S H22C 109.5 . . ?
H22A C22S H22C 109.5 . . ?
H22B C22S H22C 109.5 . . ?
F41B C23S P4B 96.7(11) . . ?
F41B C23S F45B 145(2) . . ?
P4B C23S F45B 81.2(13) . . ?
F41B C23S O2S 94.6(13) . . ?
P4B C23S O2S 162.2(11) . . ?
F45B C23S O2S 97.2(11) . . ?
F41B C23S C24S 138.8(15) . . ?
P4B C23S C24S 56.3(7) . . ?
F45B C23S C24S 67.9(12) . . ?
O2S C23S C24S 106.6(8) . . ?
F41B C23S F44B 116.7(18) . . ?
P4B C23S F44B 67.5(9) . . ?
F45B C23S F44B 95.2(14) . . ?
O2S C23S F44B 95.1(9) . . ?
C24S C23S F44B 28.7(8) . . ?
F41B C23S H23A 93.8 . . ?
P4B C23S H23A 82.5 . . ?
F45B C23S H23A 50.9 . . ?
O2S C23S H23A 110.4 . . ?
C24S C23S H23A 110.4 . . ?
F44B C23S H23A 138.6 . . ?
F41B C23S H23B 28.4 . . ?
P4B C23S H23B 75.1 . . ?
F45B C23S H23B 151.0 . . ?
O2S C23S H23B 110.4 . . ?
C24S C23S H23B 110.4 . . ?
F44B C23S H23B 91.1 . . ?
H23A C23S H23B 108.6 . . ?
F44B C24S P4B 97.2(16) . . ?
F44B C24S C23S 86(2) . . ?
P4B C24S C23S 43.8(6) . . ?
F44B C24S F45B 132(2) . . ?
P4B C24S F45B 64.6(8) . . ?
C23S C24S F45B 49.7(10) . . ?
F44B C24S F43B 125(2) . . ?
P4B C24S F43B 63.8(8) . . ?
C23S C24S F43B 105.0(9) . . ?
F45B C24S F43B 88.0(11) . . ?
F44B C24S H24A 110.7 . . ?
P4B C24S H24A 65.8 . . ?
C23S C24S H24A 109.5 . . ?
F45B C24S H24A 101.6 . . ?
F43B C24S H24A 14.7 . . ?
F44B C24S H24B 128.6 . . ?
P4B C24S H24B 128.2 . . ?
C23S C24S H24B 109.5 . . ?
F45B C24S H24B 66.4 . . ?
F43B C24S H24B 98.9 . . ?
H24A C24S H24B 109.5 . . ?
F44B C24S H24C 25.5 . . ?
P4B C24S H24C 120.9 . . ?
C23S C24S H24C 109.5 . . ?
F45B C24S H24C 147.8 . . ?
F43B C24S H24C 123.7 . . ?
H24A C24S H24C 109.5 . . ?
H24B C24S H24C 109.5 . . ?
N3S C31S C32S 175(3) . . ?
C31S C32S H32D 109.5 . . ?
C31S C32S H32E 109.5 . . ?
H32D C32S H32E 109.5 . . ?
C31S C32S H32F 109.5 . . ?
H32D C32S H32F 109.5 . . ?
H32E C32S H32F 109.5 . . ?
N3T C31T C22S 151(3) . . ?
N3T C31T C32T 174(3) . . ?
C22S C31T C32T 24.3(13) . . ?
C22S C32T C21S 105(5) . . ?
C22S C32T C31T 52(3) . . ?
C21S C32T C31T 117(3) . . ?
C22S C32T H32G 80.8 . . ?
C21S C32T H32G 124.7 . . ?
C31T C32T H32G 109.5 . . ?
C22S C32T H32H 79.8 . . ?
C21S C32T H32H 27.7 . . ?
C31T C32T H32H 109.5 . . ?
H32G C32T H32H 109.5 . . ?
C22S C32T H32I 161.7 . . ?
C21S C32T H32I 82.1 . . ?
C31T C32T H32I 109.5 . . ?
H32G C32T H32I 109.5 . . ?
H32H C32T H32I 109.5 . . ?
N1S C11S C12S 178.7(4) . . ?
C11S C12S H12A 109.5 . . ?
C11S C12S H12B 109.5 . . ?
H12A C12S H12B 109.5 . . ?
C11S C12S H12C 109.5 . . ?
H12A C12S H12C 109.5 . . ?
H12B C12S H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 -1.4(3) . . . . ?
Re1 N1 C1 C2 178.16(16) . . . . ?
N1 C1 C2 C3 -1.6(3) . . . . ?
C1 C2 C3 C4 2.9(3) . . . . ?
C1 C2 C3 C31 -179.1(2) . . . . ?
C2 C3 C31 N3 87.4(3) . . . . ?
C4 C3 C31 N3 -94.5(2) . . . . ?
C3 C31 N3 C32 -76.9(2) . . . . ?
C3 C31 N3 C33 163.96(19) . . . . ?
C3 C31 N3 C34 44.9(3) . . . . ?
C2 C3 C4 C5 -1.3(3) . . . . ?
C31 C3 C4 C5 -179.4(2) . . . . ?
C1 N1 C5 C4 3.1(3) . . . . ?
Re1 N1 C5 C4 -176.51(16) . . . . ?
C1 N1 C5 C6 -175.42(19) . . . . ?
Re1 N1 C5 C6 5.0(2) . . . . ?
C3 C4 C5 N1 -1.8(3) . . . . ?
C3 C4 C5 C6 176.6(2) . . . . ?
C10 N2 C6 C7 -0.3(3) . . . . ?
Re1 N2 C6 C7 178.67(17) . . . . ?
C10 N2 C6 C5 178.1(2) . . . . ?
Re1 N2 C6 C5 -2.9(3) . . . . ?
N1 C5 C6 N2 -1.3(3) . . . . ?
C4 C5 C6 N2 -179.8(2) . . . . ?
N1 C5 C6 C7 177.0(2) . . . . ?
C4 C5 C6 C7 -1.5(3) . . . . ?
N2 C6 C7 C8 -1.1(3) . . . . ?
C5 C6 C7 C8 -179.4(2) . . . . ?
C6 C7 C8 C9 1.9(4) . . . . ?
C6 C7 C8 C41 179.5(2) . . . . ?
C9 C8 C41 N4 -96.4(3) . . . . ?
C7 C8 C41 N4 86.0(3) . . . . ?
C8 C41 N4 C44 48.9(3) . . . . ?
C8 C41 N4 C43 168.14(19) . . . . ?
C8 C41 N4 C42 -73.3(2) . . . . ?
C7 C8 C9 C10 -1.5(4) . . . . ?
C41 C8 C9 C10 -179.1(3) . . . . ?
C6 N2 C10 C9 0.8(4) . . . . ?
Re1 N2 C10 C9 -178.1(2) . . . . ?
C8 C9 C10 N2 0.1(5) . . . . ?
C24S P4B F41B C23S 36.6(18) . . . . ?
F42B P4B F41B C23S -121.8(18) . . . . ?
F45B P4B F41B C23S -28.9(18) . . . . ?
F46B P4B F41B C23S 147.0(17) . . . . ?
F44B P4B F41B C23S 60.0(18) . . . . ?
C23S P4B F43B C24S 37.1(19) . . . . ?
F42B P4B F43B C24S 157.8(11) . . . . ?
F45B P4B F43B C24S 64.9(11) . . . . ?
F46B P4B F43B C24S -111.0(9) . . . . ?
F44B P4B F43B C24S -23.9(10) . . . . ?
C23S P4B F44B C24S -97(2) . . . . ?
F45B P4B F44B C24S -42(2) . . . . ?
F46B P4B F44B C24S 138(2) . . . . ?
F41B P4B F44B C24S -133(2) . . . . ?
F43B P4B F44B C24S 50(2) . . . . ?
C24S P4B F44B C23S 97(2) . . . . ?
F45B P4B F44B C23S 55.0(12) . . . . ?
F46B P4B F44B C23S -124.5(11) . . . . ?
F41B P4B F44B C23S -35.9(10) . . . . ?
F43B P4B F44B C23S 146.9(11) . . . . ?
C24S P4B F45B C23S -93.0(13) . . . . ?
F42B P4B F45B C23S 111.5(14) . . . . ?
F41B P4B F45B C23S 22.3(13) . . . . ?
F43B P4B F45B C23S -160.3(13) . . . . ?
F44B P4B F45B C23S -71.8(14) . . . . ?
C23S P4B F45B C24S 93.0(13) . . . . ?
F42B P4B F45B C24S -155.5(12) . . . . ?
F41B P4B F45B C24S 115.2(11) . . . . ?
F43B P4B F45B C24S -67.3(11) . . . . ?
F44B P4B F45B C24S 21.2(11) . . . . ?
C23S O2S C21S C32T -147.2(14) . . . . ?
C23S O2S C21S C22S -170.2(10) . . . . ?
O2S C21S C22S C32T 74(5) . . . . ?
C32T C21S C22S C31T -86(5) . . . . ?
O2S C21S C22S C31T -13(2) . . . . ?
P4B F41B C23S F45B 84(3) . . . . ?
P4B F41B C23S O2S -166.3(15) . . . . ?
P4B F41B C23S C24S -44.5(17) . . . . ?
P4B F41B C23S F44B -68.2(11) . . . . ?
C24S P4B C23S F41B -146.3(17) . . . . ?
F42B P4B C23S F41B 64.3(19) . . . . ?
F45B P4B C23S F41B 144(2) . . . . ?
F46B P4B C23S F41B -40.0(19) . . . . ?
F43B P4B C23S F41B 178.6(18) . . . . ?
F44B P4B C23S F41B -116.2(18) . . . . ?
C24S P4B C23S F45B 69.3(13) . . . . ?
F42B P4B C23S F45B -80.1(14) . . . . ?
F46B P4B C23S F45B 175.6(13) . . . . ?
F41B P4B C23S F45B -144(2) . . . . ?
F43B P4B C23S F45B 34(2) . . . . ?
F44B P4B C23S F45B 99.4(14) . . . . ?
C24S P4B C23S O2S -17(4) . . . . ?
F42B P4B C23S O2S -166(4) . . . . ?
F45B P4B C23S O2S -86(4) . . . . ?
F46B P4B C23S O2S 89(4) . . . . ?
F41B P4B C23S O2S 129(5) . . . . ?
F43B P4B C23S O2S -52(5) . . . . ?
F44B P4B C23S O2S 13(4) . . . . ?
F42B P4B C23S C24S -149.4(12) . . . . ?
F45B P4B C23S C24S -69.3(13) . . . . ?
F46B P4B C23S C24S 106.3(11) . . . . ?
F41B P4B C23S C24S 146.3(17) . . . . ?
F43B P4B C23S C24S -35.2(19) . . . . ?
F44B P4B C23S C24S 30.1(9) . . . . ?
C24S P4B C23S F44B -30.1(9) . . . . ?
F42B P4B C23S F44B -179.5(13) . . . . ?
F45B P4B C23S F44B -99.4(14) . . . . ?
F46B P4B C23S F44B 76.2(12) . . . . ?
F41B P4B C23S F44B 116.2(18) . . . . ?
F43B P4B C23S F44B -65(2) . . . . ?
P4B F45B C23S F41B -89(2) . . . . ?
C24S F45B C23S F41B -146(2) . . . . ?
C24S F45B C23S P4B -57.2(8) . . . . ?
P4B F45B C23S O2S 162.1(11) . . . . ?
C24S F45B C23S O2S 105.0(8) . . . . ?
P4B F45B C23S C24S 57.2(8) . . . . ?
P4B F45B C23S F44B 66.3(9) . . . . ?
C24S F45B C23S F44B 9.1(10) . . . . ?
C21S O2S C23S F41B -31.9(17) . . . . ?
C21S O2S C23S P4B -161(4) . . . . ?
C21S O2S C23S F45B 114.9(13) . . . . ?
C21S O2S C23S C24S -176.1(9) . . . . ?
C21S O2S C23S F44B -149.3(11) . . . . ?
C24S F44B C23S F41B 147(2) . . . . ?
P4B F44B C23S F41B 86.2(14) . . . . ?
C24S F44B C23S P4B 60.4(17) . . . . ?
C24S F44B C23S F45B -17.8(19) . . . . ?
P4B F44B C23S F45B -78.3(13) . . . . ?
C24S F44B C23S O2S -115.6(18) . . . . ?
P4B F44B C23S O2S -176.0(13) . . . . ?
P4B F44B C23S C24S -60.4(17) . . . . ?
C23S F44B C24S P4B -42.4(7) . . . . ?
P4B F44B C24S C23S 42.4(7) . . . . ?
P4B F44B C24S F45B 62.1(18) . . . . ?
C23S F44B C24S F45B 19.8(19) . . . . ?
P4B F44B C24S F43B -63.0(15) . . . . ?
C23S F44B C24S F43B -105.3(17) . . . . ?
C23S P4B C24S F44B 76(2) . . . . ?
F42B P4B C24S F44B -173(2) . . . . ?
F45B P4B C24S F44B 133(2) . . . . ?
F46B P4B C24S F44B -45(2) . . . . ?
F41B P4B C24S F44B 53(2) . . . . ?
F43B P4B C24S F44B -126(2) . . . . ?
F42B P4B C24S C23S 111(2) . . . . ?
F45B P4B C24S C23S 57.4(13) . . . . ?
F46B P4B C24S C23S -120.6(12) . . . . ?
F41B P4B C24S C23S -23.2(12) . . . . ?
F43B P4B C24S C23S 158.4(12) . . . . ?
F44B P4B C24S C23S -76(2) . . . . ?
C23S P4B C24S F45B -57.4(13) . . . . ?
F42B P4B C24S F45B 54(2) . . . . ?
F46B P4B C24S F45B -178.0(12) . . . . ?
F41B P4B C24S F45B -80.6(12) . . . . ?
F43B P4B C24S F45B 101.0(11) . . . . ?
F44B P4B C24S F45B -133(2) . . . . ?
C23S P4B C24S F43B -158.4(12) . . . . ?
F42B P4B C24S F43B -47(2) . . . . ?
F45B P4B C24S F43B -101.0(11) . . . . ?
F46B P4B C24S F43B 81.0(10) . . . . ?
F41B P4B C24S F43B 178.4(11) . . . . ?
F44B P4B C24S F43B 126(2) . . . . ?
F41B C23S C24S F44B -48(3) . . . . ?
P4B C23S C24S F44B -105.1(19) . . . . ?
F45B C23S C24S F44B 161(2) . . . . ?
O2S C23S C24S F44B 69.6(19) . . . . ?
F41B C23S C24S P4B 57(2) . . . . ?
F45B C23S C24S P4B -94.1(14) . . . . ?
O2S C23S C24S P4B 174.7(14) . . . . ?
F44B C23S C24S P4B 105.1(19) . . . . ?
F41B C23S C24S F45B 151(3) . . . . ?
P4B C23S C24S F45B 94.1(14) . . . . ?
O2S C23S C24S F45B -91.2(13) . . . . ?
F44B C23S C24S F45B -161(2) . . . . ?
F41B C23S C24S F43B 77(3) . . . . ?
P4B C23S C24S F43B 20.0(11) . . . . ?
F45B C23S C24S F43B -74.1(13) . . . . ?
O2S C23S C24S F43B -165.3(10) . . . . ?
F44B C23S C24S F43B 125(2) . . . . ?
C23S F45B C24S F44B -26(3) . . . . ?
P4B F45B C24S F44B -76(2) . . . . ?
C23S F45B C24S P4B 49.8(8) . . . . ?
P4B F45B C24S C23S -49.8(8) . . . . ?
C23S F45B C24S F43B 111.6(10) . . . . ?
P4B F45B C24S F43B 61.8(8) . . . . ?
P4B F43B C24S F44B 80(2) . . . . ?
P4B F43B C24S C23S -15.3(8) . . . . ?
P4B F43B C24S F45B -62.6(9) . . . . ?
C32T C22S C31T N3T -169(6) . . . . ?
C21S C22S C31T N3T -116(5) . . . . ?
C21S C22S C31T C32T 53(4) . . . . ?
C31T C22S C32T C21S 113(3) . . . . ?
C21S C22S C32T C31T -113(3) . . . . ?
O2S C21S C32T C22S -109(5) . . . . ?
C22S C21S C32T C31T 55(3) . . . . ?
O2S C21S C32T C31T -55(3) . . . . ?
C22S C31T C32T C21S -88(5) . . . . ?

_refine_diff_density_max         1.432
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.150



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Et2O/MeCN+ tetrabutylammonium hexafluorophosphate'
####################################################################### 
# 
# 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_V18105
_database_code_depnum_ccdc_archive 'CCDC 2494314'
loop_
_audit_author_name
_audit_author_address
'Michael K. Takase'
;California Institute of Technology
United States of America
;
_audit_update_record             
;
2025-10-15 deposited with the CCDC.	2026-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21H28BrReN4O32+ 2(F6P-) 0.5(H3C2N)'
_chemical_formula_sum            'C22 H29.50 Cl F12 N4.50 O3 P2 Re'
_chemical_formula_weight         916.59

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'
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                   18.1497(10)
_cell_length_b                   13.5754(9)
_cell_length_c                   12.6756(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.113(3)
_cell_angle_gamma                90
_cell_volume                     3105.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9864
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      35.76

_exptl_crystal_description       Block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_F_000             1788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.209
_shelx_estimated_absorpt_T_min   0.678
_shelx_estimated_absorpt_T_max   0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6427
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 7.69
_diffrn_reflns_number            42554
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.257
_diffrn_reflns_theta_max         36.321
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             14868
_reflns_number_gt                10894
_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       'APEX3 v2017.3-0 (Bruker-AXS, 2017)'
_computing_cell_refinement       'SAINT v8.38A (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT v8.38A (Bruker-AXS, 2013)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²+7.3261P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14868
_refine_ls_number_parameters     431
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1007
_refine_ls_wR_factor_gt          0.0897
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
Cl1 Cl 0.44960(6) 0.76764(10) 0.46096(8) 0.0463(3) Uani 1 1 d . . . . .
Re1 Re 0.39046(2) 0.69741(2) 0.29150(2) 0.02597(4) Uani 1 1 d . . . . .
N1 N 0.28995(15) 0.7180(2) 0.3688(2) 0.0275(6) Uani 1 1 d . . . . .
C1 C 0.24889(19) 0.8000(3) 0.3629(3) 0.0316(8) Uani 1 1 d . . . . .
H1 H 0.259538 0.849942 0.314198 0.038 Uiso 1 1 calc R U . . .
C2 C 0.19157(19) 0.8152(3) 0.4247(3) 0.0281(7) Uani 1 1 d . . . . .
H2 H 0.163992 0.874821 0.418898 0.034 Uiso 1 1 calc R U . . .
C3 C 0.17473(17) 0.7425(2) 0.4955(2) 0.0218(5) Uani 1 1 d . . . . .
C11 C 0.11667(18) 0.7576(2) 0.5708(3) 0.0233(6) Uani 1 1 d . . . . .
H11A H 0.117537 0.827527 0.592961 0.028 Uiso 1 1 calc R U . . .
H11B H 0.130039 0.717238 0.635017 0.028 Uiso 1 1 calc R U . . .
N3 N 0.03841(15) 0.7313(2) 0.5255(2) 0.0260(6) Uani 1 1 d . . . . .
C13 C 0.0116(3) 0.7980(4) 0.4360(4) 0.0507(12) Uani 1 1 d . . . . .
H13A H 0.044826 0.793327 0.380181 0.076 Uiso 1 1 calc R U . . .
H13B H 0.010823 0.866043 0.461779 0.076 Uiso 1 1 calc R U . . .
H13C H -0.038577 0.778498 0.407314 0.076 Uiso 1 1 calc R U . . .
C14 C -0.0091(3) 0.7445(4) 0.6140(4) 0.0507(12) Uani 1 1 d . . . . .
H14A H -0.060716 0.729769 0.588362 0.076 Uiso 1 1 calc R U . . .
H14B H -0.005271 0.812734 0.639401 0.076 Uiso 1 1 calc R U . . .
H14C H 0.007745 0.699763 0.672332 0.076 Uiso 1 1 calc R U . . .
C15 C 0.0337(2) 0.6274(3) 0.4893(3) 0.0364(8) Uani 1 1 d . . . . .
H15A H 0.051855 0.583939 0.548065 0.055 Uiso 1 1 calc R U . . .
H15B H 0.064067 0.618576 0.430505 0.055 Uiso 1 1 calc R U . . .
H15C H -0.017977 0.611076 0.465233 0.055 Uiso 1 1 calc R U . . .
C4 C 0.21690(16) 0.6573(2) 0.5012(2) 0.0209(5) Uani 1 1 d . . . . .
H4 H 0.206754 0.606220 0.548857 0.025 Uiso 1 1 calc R U . . .
C5 C 0.27412(16) 0.6463(2) 0.4373(2) 0.0218(6) Uani 1 1 d . . . . .
C6 C 0.32215(17) 0.5587(2) 0.4412(2) 0.0225(6) Uani 1 1 d . . . . .
C7 C 0.30952(17) 0.4759(2) 0.5006(2) 0.0220(6) Uani 1 1 d . . . . .
H7 H 0.268213 0.473880 0.540684 0.026 Uiso 1 1 calc R U . . .
C8 C 0.35717(17) 0.3959(3) 0.5015(3) 0.0238(6) Uani 1 1 d . . . . .
C16 C 0.3449(2) 0.3070(2) 0.5685(3) 0.0259(6) Uani 1 1 d . . . . .
H16A H 0.321186 0.328551 0.631436 0.031 Uiso 1 1 calc R U . . .
H16B H 0.393625 0.278149 0.594049 0.031 Uiso 1 1 calc R U . . .
N4 N 0.29733(18) 0.2281(2) 0.5113(2) 0.0302(6) Uani 1 1 d . . . . .
C18 C 0.2248(2) 0.2672(3) 0.4655(4) 0.0423(10) Uani 1 1 d . . . . .
H18A H 0.231776 0.309635 0.404889 0.063 Uiso 1 1 calc R U . . .
H18B H 0.202458 0.305474 0.519489 0.063 Uiso 1 1 calc R U . . .
H18C H 0.191961 0.212315 0.441981 0.063 Uiso 1 1 calc R U . . .
C19 C 0.2850(4) 0.1492(3) 0.5914(4) 0.0633(17) Uani 1 1 d . . . . .
H19A H 0.257279 0.176843 0.646677 0.095 Uiso 1 1 calc R U . . .
H19B H 0.332953 0.124576 0.623592 0.095 Uiso 1 1 calc R U . . .
H19C H 0.256717 0.094854 0.555879 0.095 Uiso 1 1 calc R U . . .
C20 C 0.3365(2) 0.1828(3) 0.4251(3) 0.0376(9) Uani 1 1 d . . . . .
H20A H 0.306659 0.128563 0.392334 0.056 Uiso 1 1 calc R U . . .
H20B H 0.384799 0.157567 0.455224 0.056 Uiso 1 1 calc R U . . .
H20C H 0.343716 0.232706 0.371224 0.056 Uiso 1 1 calc R U . . .
C9 C 0.41739(19) 0.4027(3) 0.4417(3) 0.0333(8) Uani 1 1 d . . . . .
H9 H 0.451952 0.350176 0.441390 0.040 Uiso 1 1 calc R U . . .
C10 C 0.4259(2) 0.4866(3) 0.3833(4) 0.0379(9) Uani 1 1 d . . . . .
H10 H 0.466390 0.490084 0.341852 0.046 Uiso 1 1 calc R U . . .
N2 N 0.37992(15) 0.5633(2) 0.3822(2) 0.0291(6) Uani 1 1 d . . . . .
C21 C 0.3405(2) 0.6372(3) 0.1642(3) 0.0334(8) Uani 1 1 d . . . . .
O1 O 0.31399(17) 0.6018(3) 0.0914(3) 0.0478(8) Uani 1 1 d . . . . .
C22 C 0.4841(2) 0.6686(3) 0.2425(3) 0.0318(7) Uani 1 1 d . . . . .
O2 O 0.54127(15) 0.6499(3) 0.2169(2) 0.0434(7) Uani 1 1 d . . . . .
C23 C 0.3940(2) 0.8220(3) 0.2201(3) 0.0304(7) Uani 1 1 d . . . . .
O3 O 0.39695(16) 0.8981(2) 0.1802(2) 0.0404(7) Uani 1 1 d . . . . .
P1 P 0.12981(6) 0.47765(7) 0.24376(7) 0.02889(18) Uani 1 1 d . . . . .
F11 F 0.04265(17) 0.4714(3) 0.2324(3) 0.0846(12) Uani 1 1 d . . . . .
F12 F 0.1259(2) 0.59328(19) 0.2653(2) 0.0632(9) Uani 1 1 d . . . . .
F13 F 0.13220(17) 0.4609(2) 0.36943(18) 0.0479(6) Uani 1 1 d . . . . .
F14 F 0.1292(2) 0.4962(2) 0.11976(19) 0.0624(9) Uani 1 1 d . . . . .
F15 F 0.13323(16) 0.36221(18) 0.2242(2) 0.0463(6) Uani 1 1 d . . . . .
F16 F 0.21831(15) 0.4807(2) 0.2579(2) 0.0572(8) Uani 1 1 d . . . . .
P2 P 0.15960(5) 0.44409(6) 0.73202(6) 0.02254(16) Uani 1 1 d . . . . .
F21 F 0.08358(14) 0.38796(19) 0.7370(2) 0.0432(6) Uani 1 1 d . . . . .
F22 F 0.17299(15) 0.44745(17) 0.85853(16) 0.0387(5) Uani 1 1 d . . . . .
F23 F 0.11871(13) 0.54885(16) 0.73181(17) 0.0328(5) Uani 1 1 d . . . . .
F24 F 0.14656(11) 0.44196(16) 0.60420(15) 0.0279(4) Uani 1 1 d . . . . .
F25 F 0.20272(15) 0.34110(17) 0.73064(18) 0.0387(5) Uani 1 1 d . . . . .
F26 F 0.23690(12) 0.49974(18) 0.72488(18) 0.0366(5) Uani 1 1 d . . . . .
N1S N 0.4426(8) 0.4104(13) 0.1694(12) 0.108(6) Uani 0.5 1 d . . P A -1
C11S C 0.4731(10) 0.4472(11) 0.1112(14) 0.077(4) Uani 0.5 1 d . . P A -1
C12S C 0.5197(17) 0.4856(11) 0.0412(18) 0.153(11) Uani 0.5 1 d . . P A -1
H12A H 0.570413 0.489231 0.076474 0.230 Uiso 0.5 1 calc R U P A -1
H12B H 0.502899 0.551770 0.019121 0.230 Uiso 0.5 1 calc R U P A -1
H12C H 0.518775 0.442885 -0.021239 0.230 Uiso 0.5 1 calc 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
Cl1 Re1 2.4868(12) . ?
Re1 C22 1.911(4) . ?
Re1 C23 1.923(4) . ?
Re1 C21 1.944(5) . ?
Re1 N2 2.173(3) . ?
Re1 N1 2.178(3) . ?
N1 C1 1.338(4) . ?
N1 C5 1.356(4) . ?
C1 C2 1.383(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.389(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(4) . ?
C3 C11 1.509(4) . ?
C11 N3 1.516(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N3 C15 1.483(5) . ?
N3 C13 1.492(5) . ?
N3 C14 1.496(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C4 C5 1.391(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.472(4) . ?
C6 N2 1.352(4) . ?
C6 C7 1.386(4) . ?
C7 C8 1.387(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.398(5) . ?
C8 C16 1.506(5) . ?
C16 N4 1.512(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
N4 C18 1.480(5) . ?
N4 C20 1.498(4) . ?
N4 C19 1.509(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C9 C10 1.376(5) . ?
C9 H9 0.9500 . ?
C10 N2 1.333(5) . ?
C10 H10 0.9500 . ?
C21 O1 1.105(5) . ?
C22 O2 1.148(4) . ?
C23 O3 1.153(4) . ?
P1 F11 1.575(3) . ?
P1 F15 1.589(3) . ?
P1 F14 1.591(3) . ?
P1 F12 1.596(3) . ?
P1 F16 1.598(3) . ?
P1 F13 1.605(2) . ?
P2 F21 1.583(2) . ?
P2 F22 1.597(2) . ?
P2 F25 1.603(2) . ?
P2 F23 1.604(2) . ?
P2 F26 1.605(2) . ?
P2 F24 1.613(2) . ?
N1S C11S 1.09(2) . ?
C11S C12S 1.39(3) . ?
C12S H12A 0.9800 . ?
C12S H12B 0.9800 . ?
C12S H12C 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
C22 Re1 C23 87.27(16) . . ?
C22 Re1 C21 89.81(16) . . ?
C23 Re1 C21 90.87(16) . . ?
C22 Re1 N2 97.58(14) . . ?
C23 Re1 N2 174.58(13) . . ?
C21 Re1 N2 91.57(14) . . ?
C22 Re1 N1 171.37(14) . . ?
C23 Re1 N1 99.76(13) . . ?
C21 Re1 N1 95.04(14) . . ?
N2 Re1 N1 75.20(10) . . ?
C22 Re1 Cl1 92.43(12) . . ?
C23 Re1 Cl1 92.07(12) . . ?
C21 Re1 Cl1 176.38(11) . . ?
N2 Re1 Cl1 85.32(10) . . ?
N1 Re1 Cl1 82.39(9) . . ?
C1 N1 C5 118.6(3) . . ?
C1 N1 Re1 124.8(2) . . ?
C5 N1 Re1 116.2(2) . . ?
N1 C1 C2 122.7(3) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C1 C2 C3 119.4(3) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 118.0(3) . . ?
C4 C3 C11 119.9(3) . . ?
C2 C3 C11 121.9(3) . . ?
C3 C11 N3 114.7(3) . . ?
C3 C11 H11A 108.6 . . ?
N3 C11 H11A 108.6 . . ?
C3 C11 H11B 108.6 . . ?
N3 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
C15 N3 C13 109.8(3) . . ?
C15 N3 C14 109.1(3) . . ?
C13 N3 C14 109.3(3) . . ?
C15 N3 C11 111.2(3) . . ?
C13 N3 C11 111.2(3) . . ?
C14 N3 C11 106.2(3) . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C14 H14A 109.5 . . ?
N3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C3 C4 C5 120.1(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 121.2(3) . . ?
N1 C5 C6 115.8(3) . . ?
C4 C5 C6 122.9(3) . . ?
N2 C6 C7 121.3(3) . . ?
N2 C6 C5 115.9(3) . . ?
C7 C6 C5 122.8(3) . . ?
C6 C7 C8 120.0(3) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 117.8(3) . . ?
C7 C8 C16 120.2(3) . . ?
C9 C8 C16 122.0(3) . . ?
C8 C16 N4 114.1(3) . . ?
C8 C16 H16A 108.7 . . ?
N4 C16 H16A 108.7 . . ?
C8 C16 H16B 108.7 . . ?
N4 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C18 N4 C20 109.5(3) . . ?
C18 N4 C19 109.2(4) . . ?
C20 N4 C19 108.4(3) . . ?
C18 N4 C16 111.9(3) . . ?
C20 N4 C16 110.5(3) . . ?
C19 N4 C16 107.4(3) . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 H19A 109.5 . . ?
N4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C20 H20A 109.5 . . ?
N4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C10 C9 C8 119.0(3) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
N2 C10 C9 123.2(3) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
C10 N2 C6 118.6(3) . . ?
C10 N2 Re1 124.7(2) . . ?
C6 N2 Re1 116.6(2) . . ?
O1 C21 Re1 177.9(4) . . ?
O2 C22 Re1 177.4(4) . . ?
O3 C23 Re1 177.9(4) . . ?
F11 P1 F15 89.33(19) . . ?
F11 P1 F14 90.9(2) . . ?
F15 P1 F14 89.90(15) . . ?
F11 P1 F12 90.3(2) . . ?
F15 P1 F12 179.04(16) . . ?
F14 P1 F12 91.01(14) . . ?
F11 P1 F16 178.0(2) . . ?
F15 P1 F16 89.29(16) . . ?
F14 P1 F16 90.46(18) . . ?
F12 P1 F16 91.02(19) . . ?
F11 P1 F13 90.23(19) . . ?
F15 P1 F13 91.01(15) . . ?
F14 P1 F13 178.53(19) . . ?
F12 P1 F13 88.09(14) . . ?
F16 P1 F13 88.40(16) . . ?
F21 P2 F22 90.82(14) . . ?
F21 P2 F25 90.53(14) . . ?
F22 P2 F25 90.78(12) . . ?
F21 P2 F23 91.25(14) . . ?
F22 P2 F23 89.85(12) . . ?
F25 P2 F23 178.11(13) . . ?
F21 P2 F26 178.83(13) . . ?
F22 P2 F26 90.15(14) . . ?
F25 P2 F26 88.81(14) . . ?
F23 P2 F26 89.40(13) . . ?
F21 P2 F24 89.76(12) . . ?
F22 P2 F24 179.31(14) . . ?
F25 P2 F24 89.60(12) . . ?
F23 P2 F24 89.76(12) . . ?
F26 P2 F24 89.27(11) . . ?
N1S C11S C12S 172(2) . . ?
C11S C12S H12A 109.5 . . ?
C11S C12S H12B 109.5 . . ?
H12A C12S H12B 109.5 . . ?
C11S C12S H12C 109.5 . . ?
H12A C12S H12C 109.5 . . ?
H12B C12S H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 0.8(6) . . . . ?
Re1 N1 C1 C2 -170.7(3) . . . . ?
N1 C1 C2 C3 -0.7(6) . . . . ?
C1 C2 C3 C4 0.3(5) . . . . ?
C1 C2 C3 C11 175.4(3) . . . . ?
C4 C3 C11 N3 -97.7(4) . . . . ?
C2 C3 C11 N3 87.3(4) . . . . ?
C3 C11 N3 C15 57.5(4) . . . . ?
C3 C11 N3 C13 -65.1(4) . . . . ?
C3 C11 N3 C14 176.1(3) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
C11 C3 C4 C5 -175.2(3) . . . . ?
C1 N1 C5 C4 -0.5(5) . . . . ?
Re1 N1 C5 C4 171.8(3) . . . . ?
C1 N1 C5 C6 -179.0(3) . . . . ?
Re1 N1 C5 C6 -6.8(4) . . . . ?
C3 C4 C5 N1 0.1(5) . . . . ?
C3 C4 C5 C6 178.6(3) . . . . ?
N1 C5 C6 N2 5.0(5) . . . . ?
C4 C5 C6 N2 -173.5(3) . . . . ?
N1 C5 C6 C7 -174.6(3) . . . . ?
C4 C5 C6 C7 6.9(5) . . . . ?
N2 C6 C7 C8 0.9(5) . . . . ?
C5 C6 C7 C8 -179.5(3) . . . . ?
C6 C7 C8 C9 0.4(5) . . . . ?
C6 C7 C8 C16 178.2(3) . . . . ?
C7 C8 C16 N4 91.6(4) . . . . ?
C9 C8 C16 N4 -90.7(4) . . . . ?
C8 C16 N4 C18 -55.4(4) . . . . ?
C8 C16 N4 C20 66.9(4) . . . . ?
C8 C16 N4 C19 -175.1(3) . . . . ?
C7 C8 C9 C10 -1.4(6) . . . . ?
C16 C8 C9 C10 -179.1(4) . . . . ?
C8 C9 C10 N2 1.2(7) . . . . ?
C9 C10 N2 C6 0.0(7) . . . . ?
C9 C10 N2 Re1 -179.9(3) . . . . ?
C7 C6 N2 C10 -1.1(6) . . . . ?
C5 C6 N2 C10 179.3(4) . . . . ?
C7 C6 N2 Re1 178.9(3) . . . . ?
C5 C6 N2 Re1 -0.8(4) . . . . ?

_refine_diff_density_max         4.880
_refine_diff_density_min         -2.659
_refine_diff_density_rms         0.155



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Et2O/MeCN'
