# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1484945'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-07-05 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C35 H23 F6 N8 O Os P, C H2 Cl2'
_chemical_formula_sum            'C36 H25 Cl2 F6 N8 O Os P'
_chemical_formula_weight         991.71
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 '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'

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '
_symmetry_space_group_name_Hall  '-P 1 '
_cell_length_a                   10.8160(5)
_cell_length_b                   13.4759(6)
_cell_length_c                   14.5272(6)
_cell_angle_alpha                62.8130(10)
_cell_angle_beta                 89.808(2)
_cell_angle_gamma                84.357(2)
_cell_volume                     1872.29(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6465
_cell_measurement_temperature    171(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      3.16
_exptl_absorpt_coefficient_mu    3.663
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15234
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         3.16
_diffrn_ambient_temperature      171(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_reflns_number_gt                5647
_reflns_number_total             6639
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    ?
_computing_publication_material  ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6639
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0317
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0301P)²+1.2335P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0669
_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. 
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7622(4) 0.5939(4) 0.0296(3) 0.0174(10) Uani 1 1 d . . .
C2 C 0.6171(4) 0.6815(4) -0.0780(3) 0.0185(10) Uani 1 1 d . . .
C3 C 0.8676(4) 0.5210(4) 0.0962(3) 0.0169(10) Uani 1 1 d . . .
C4 C 0.9161(4) 0.4223(4) 0.0957(4) 0.0240(11) Uani 1 1 d . . .
H4 H 0.8790 0.3967 0.0524 0.029 Uiso 1 1 calc R . .
C5 C 1.0198(5) 0.3617(4) 0.1594(4) 0.0270(12) Uani 1 1 d . . .
H5 H 1.0549 0.2936 0.1607 0.032 Uiso 1 1 calc R . .
C6 C 1.0711(5) 0.4016(4) 0.2209(4) 0.0262(12) Uani 1 1 d . . .
H6 H 1.1428 0.3614 0.2644 0.031 Uiso 1 1 calc R . .
C7 C 1.0187(4) 0.4989(4) 0.2194(4) 0.0205(10) Uani 1 1 d . . .
H7 H 1.0547 0.5246 0.2630 0.025 Uiso 1 1 calc R . .
C8 C 0.5183(5) 0.7097(4) -0.1594(4) 0.0276(12) Uani 1 1 d . . .
C9 C 0.8917(4) 0.9183(4) -0.0302(3) 0.0196(10) Uani 1 1 d . . .
C10 C 1.0333(4) 0.8898(4) -0.1141(4) 0.0223(11) Uani 1 1 d . . .
C11 C 0.7862(4) 0.9581(4) 0.0106(3) 0.0202(10) Uani 1 1 d . . .
C12 C 0.7355(5) 1.0688(4) -0.0328(4) 0.0277(12) Uani 1 1 d . . .
H12 H 0.7724 1.1242 -0.0905 0.033 Uiso 1 1 calc R . .
C13 C 0.6308(5) 1.0991(4) 0.0076(4) 0.0298(12) Uani 1 1 d . . .
H13 H 0.5963 1.1753 -0.0201 0.036 Uiso 1 1 calc R . .
C14 C 0.5784(4) 1.0163(4) 0.0886(4) 0.0250(12) Uani 1 1 d . . .
H14 H 0.5048 1.0340 0.1164 0.030 Uiso 1 1 calc R . .
C15 C 0.6332(4) 0.9063(4) 0.1299(3) 0.0185(10) Uani 1 1 d . . .
H15 H 0.5957 0.8499 0.1862 0.022 Uiso 1 1 calc R . .
C16 C 1.1198(5) 0.9084(4) -0.1986(4) 0.0326(13) Uani 1 1 d . . .
C17 C 0.5431(4) 0.6202(3) 0.2521(3) 0.0159(10) Uani 1 1 d . . .
C18 C 0.5085(4) 0.5836(4) 0.1809(3) 0.0219(11) Uani 1 1 d . . .
H18 H 0.5708 0.5520 0.1527 0.026 Uiso 1 1 calc R . .
C19 C 0.3846(4) 0.5928(4) 0.1508(4) 0.0257(11) Uani 1 1 d . . .
H19 H 0.3623 0.5665 0.1033 0.031 Uiso 1 1 calc R . .
C20 C 0.2945(4) 0.6399(4) 0.1898(4) 0.0282(12) Uani 1 1 d . . .
H20 H 0.2099 0.6478 0.1678 0.034 Uiso 1 1 calc R . .
C21 C 0.3256(5) 0.6761(4) 0.2608(4) 0.0288(12) Uani 1 1 d . . .
H21 H 0.2625 0.7077 0.2882 0.035 Uiso 1 1 calc R . .
C22 C 0.4485(4) 0.6664(4) 0.2916(4) 0.0219(11) Uani 1 1 d . . .
H22 H 0.4694 0.6914 0.3404 0.026 Uiso 1 1 calc R . .
C23 C 0.7641(4) 0.4651(4) 0.3593(3) 0.0216(11) Uani 1 1 d . . .
C24 C 0.8711(5) 0.4364(4) 0.4235(4) 0.0332(13) Uani 1 1 d . . .
H24 H 0.9077 0.4928 0.4325 0.040 Uiso 1 1 calc R . .
C25 C 0.9241(6) 0.3261(5) 0.4742(4) 0.0489(18) Uani 1 1 d . . .
H25 H 0.9964 0.3074 0.5183 0.059 Uiso 1 1 calc R . .
C26 C 0.8737(7) 0.2438(5) 0.4615(5) 0.063(2) Uani 1 1 d . . .
H26 H 0.9109 0.1683 0.4961 0.075 Uiso 1 1 calc R . .
C27 C 0.7678(7) 0.2714(5) 0.3978(6) 0.071(2) Uani 1 1 d . . .
H27 H 0.7320 0.2148 0.3885 0.085 Uiso 1 1 calc R . .
C28 C 0.7145(6) 0.3808(4) 0.3479(5) 0.0421(15) Uani 1 1 d . . .
H28 H 0.6417 0.3987 0.3046 0.050 Uiso 1 1 calc R . .
C29 C 0.7025(4) 0.6576(4) 0.3889(3) 0.0199(10) Uani 1 1 d . . .
C30 C 0.7371(4) 0.7601(4) 0.3727(3) 0.0189(10) Uani 1 1 d . . .
H30 H 0.7703 0.8073 0.3085 0.023 Uiso 1 1 calc R . .
C31 C 0.7243(5) 0.7953(4) 0.4484(4) 0.0271(12) Uani 1 1 d . . .
H31 H 0.7489 0.8659 0.4362 0.032 Uiso 1 1 calc R . .
C32 C 0.6759(5) 0.7278(4) 0.5416(4) 0.0310(13) Uani 1 1 d . . .
H32 H 0.6654 0.7523 0.5933 0.037 Uiso 1 1 calc R . .
C33 C 0.6425(5) 0.6237(4) 0.5597(4) 0.0312(13) Uani 1 1 d . . .
H33 H 0.6109 0.5764 0.6246 0.037 Uiso 1 1 calc R . .
C34 C 0.6547(4) 0.5887(4) 0.4845(4) 0.0245(11) Uani 1 1 d . . .
H34 H 0.6307 0.5177 0.4973 0.029 Uiso 1 1 calc R . .
C35 C 0.9456(4) 0.7224(4) 0.2359(4) 0.0216(11) Uani 1 1 d . . .
C36 C 0.7221(7) 0.9953(7) 0.7157(6) 0.082(3) Uani 1 1 d . . .
H36A H 0.7050 0.9447 0.7884 0.098 Uiso 1 1 calc R . .
H36B H 0.7891 1.0399 0.7166 0.098 Uiso 1 1 calc R . .
Cl1 Cl 0.5903(2) 1.08453(18) 0.65571(18) 0.0908(7) Uani 1 1 d . . .
Cl2 Cl 0.7731(2) 0.9149(2) 0.6547(3) 0.1238(11) Uani 1 1 d . . .
F1 F 0.5590(3) 0.6890(3) -0.2363(2) 0.0472(9) Uani 1 1 d . . .
F2 F 0.4223(3) 0.6490(3) -0.1230(2) 0.0468(9) Uani 1 1 d . . .
F3 F 0.4734(3) 0.8171(3) -0.2019(2) 0.0472(9) Uani 1 1 d . . .
F4 F 1.1827(3) 0.9945(3) -0.2212(3) 0.0533(10) Uani 1 1 d . . .
F5 F 1.0623(4) 0.9242(5) -0.2843(3) 0.0903(16) Uani 1 1 d . . .
F6 F 1.2041(4) 0.8210(3) -0.1737(3) 0.0818(15) Uani 1 1 d . . .
N1 N 0.6314(3) 0.7468(3) -0.0330(3) 0.0188(9) Uani 1 1 d . . .
N2 N 0.7268(3) 0.6884(3) 0.0379(3) 0.0157(8) Uani 1 1 d . . .
N3 N 0.6956(3) 0.5855(3) -0.0432(3) 0.0197(9) Uani 1 1 d . . .
N4 N 0.9175(3) 0.5599(3) 0.1581(3) 0.0176(9) Uani 1 1 d . . .
N5 N 1.0241(3) 0.7881(3) -0.0354(3) 0.0224(9) Uani 1 1 d . . .
N6 N 0.9307(3) 0.8089(3) 0.0175(3) 0.0177(9) Uani 1 1 d . . .
N7 N 0.9535(4) 0.9743(3) -0.1161(3) 0.0252(10) Uani 1 1 d . . .
N8 N 0.7368(3) 0.8762(3) 0.0937(3) 0.0155(8) Uani 1 1 d . . .
O1 O 1.0228(3) 0.7259(3) 0.2894(3) 0.0346(9) Uani 1 1 d . . .
Os1 Os 0.831227(17) 0.712005(15) 0.146542(14) 0.01451(6) Uani 1 1 d . . .
P1 P 0.70830(11) 0.61466(9) 0.28595(9) 0.0157(3) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.456(6) . ?
C1 N2 1.352(5) . ?
C1 N3 1.334(6) . ?
C2 C8 1.484(7) . ?
C2 N1 1.334(6) . ?
C2 N3 1.356(5) . ?
C3 C4 1.384(6) . ?
C3 N4 1.365(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.385(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.377(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.367(6) . ?
C7 H7 0.9500 . ?
C7 N4 1.352(5) . ?
C8 F1 1.334(6) . ?
C8 F2 1.340(6) . ?
C8 F3 1.327(5) . ?
C9 C11 1.451(6) . ?
C9 N6 1.333(5) . ?
C9 N7 1.344(6) . ?
C10 C16 1.485(7) . ?
C10 N5 1.338(6) . ?
C10 N7 1.349(6) . ?
C11 C12 1.380(6) . ?
C11 N8 1.362(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.385(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.368(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.387(6) . ?
C15 H15 0.9500 . ?
C15 N8 1.341(5) . ?
C16 F4 1.313(6) . ?
C16 F5 1.311(6) . ?
C16 F6 1.323(6) . ?
C17 C18 1.399(6) . ?
C17 C22 1.401(6) . ?
C17 P1 1.841(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(7) . ?
C19 H19 0.9500 . ?
C19 C20 1.370(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.381(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.379(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.396(7) . ?
C23 C28 1.377(8) . ?
C23 P1 1.834(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.383(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.367(10) . ?
C26 H26 0.9500 . ?
C26 C27 1.384(10) . ?
C27 H27 0.9500 . ?
C27 C28 1.375(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.381(6) . ?
C29 C34 1.404(6) . ?
C29 P1 1.833(5) . ?
C30 H30 0.9500 . ?
C30 C31 1.384(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.378(7) . ?
C32 H32 0.9500 . ?
C32 C33 1.388(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.376(7) . ?
C34 H34 0.9500 . ?
C35 O1 1.161(6) . ?
C35 Os1 1.857(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 Cl1 1.718(7) . ?
C36 Cl2 1.737(8) . ?
N1 N2 1.361(5) . ?
N2 Os1 2.100(4) . ?
N4 Os1 2.100(4) . ?
N5 N6 1.352(5) . ?
N6 Os1 2.098(4) . ?
N8 Os1 2.130(3) . ?
Os1 P1 2.3425(12) . ?

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
N2 C1 C3 116.6(4) . . ?
N3 C1 C3 130.4(4) . . ?
N3 C1 N2 112.9(4) . . ?
N1 C2 C8 122.2(4) . . ?
N1 C2 N3 116.4(4) . . ?
N3 C2 C8 121.4(4) . . ?
C4 C3 C1 123.5(4) . . ?
N4 C3 C1 114.1(4) . . ?
N4 C3 C4 122.4(4) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 C3 118.7(5) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 H5 120.5 . . ?
C6 C5 C4 119.0(4) . . ?
C6 C5 H5 120.5 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.0(4) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 118.8 . . ?
N4 C7 C6 122.4(5) . . ?
N4 C7 H7 118.8 . . ?
F1 C8 C2 112.3(4) . . ?
F1 C8 F2 105.3(4) . . ?
F2 C8 C2 112.4(4) . . ?
F3 C8 C2 112.2(4) . . ?
F3 C8 F1 106.9(4) . . ?
F3 C8 F2 107.4(4) . . ?
N6 C9 C11 117.9(4) . . ?
N6 C9 N7 112.4(4) . . ?
N7 C9 C11 129.5(4) . . ?
N5 C10 C16 122.4(4) . . ?
N5 C10 N7 116.1(4) . . ?
N7 C10 C16 121.3(4) . . ?
C12 C11 C9 123.5(4) . . ?
N8 C11 C9 114.5(4) . . ?
N8 C11 C12 121.9(4) . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0(4) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 120.9 . . ?
C14 C13 C12 118.1(4) . . ?
C14 C13 H13 120.9 . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.7(4) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 118.6 . . ?
N8 C15 C14 122.8(4) . . ?
N8 C15 H15 118.6 . . ?
F4 C16 C10 113.0(5) . . ?
F4 C16 F6 105.7(5) . . ?
F5 C16 C10 112.4(4) . . ?
F5 C16 F4 107.5(5) . . ?
F5 C16 F6 106.0(5) . . ?
F6 C16 C10 111.7(4) . . ?
C18 C17 C22 117.8(4) . . ?
C18 C17 P1 120.5(3) . . ?
C22 C17 P1 121.7(4) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 C17 120.9(4) . . ?
C19 C18 H18 119.5 . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.9(5) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.7 . . ?
C19 C20 C21 120.6(5) . . ?
C21 C20 H20 119.7 . . ?
C20 C21 H21 120.1 . . ?
C22 C21 C20 119.8(5) . . ?
C22 C21 H21 120.1 . . ?
C17 C22 H22 119.5 . . ?
C21 C22 C17 121.0(5) . . ?
C21 C22 H22 119.5 . . ?
C24 C23 P1 117.4(4) . . ?
C28 C23 C24 118.0(5) . . ?
C28 C23 P1 124.4(4) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.3(6) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.6 . . ?
C26 C25 C24 120.8(6) . . ?
C26 C25 H25 119.6 . . ?
C25 C26 H26 120.3 . . ?
C25 C26 C27 119.3(6) . . ?
C27 C26 H26 120.3 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0(7) . . ?
C28 C27 H27 120.0 . . ?
C23 C28 H28 119.2 . . ?
C27 C28 C23 121.6(6) . . ?
C27 C28 H28 119.2 . . ?
C30 C29 C34 118.6(4) . . ?
C30 C29 P1 121.5(3) . . ?
C34 C29 P1 119.8(4) . . ?
C29 C30 H30 119.5 . . ?
C29 C30 C31 121.1(4) . . ?
C31 C30 H30 119.5 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 119.9(5) . . ?
C32 C31 H31 120.0 . . ?
C31 C32 H32 120.2 . . ?
C31 C32 C33 119.7(5) . . ?
C33 C32 H32 120.2 . . ?
C32 C33 H33 119.7 . . ?
C34 C33 C32 120.5(4) . . ?
C34 C33 H33 119.7 . . ?
C29 C34 H34 119.9 . . ?
C33 C34 C29 120.1(5) . . ?
C33 C34 H34 119.9 . . ?
O1 C35 Os1 175.8(4) . . ?
H36A C36 H36B 107.8 . . ?
Cl1 C36 H36A 109.0 . . ?
Cl1 C36 H36B 109.0 . . ?
Cl1 C36 Cl2 112.7(5) . . ?
Cl2 C36 H36A 109.0 . . ?
Cl2 C36 H36B 109.0 . . ?
C2 N1 N2 102.7(3) . . ?
C1 N2 N1 107.7(4) . . ?
C1 N2 Os1 115.6(3) . . ?
N1 N2 Os1 136.6(3) . . ?
C1 N3 C2 100.3(4) . . ?
C3 N4 Os1 116.5(3) . . ?
C7 N4 C3 117.5(4) . . ?
C7 N4 Os1 125.9(3) . . ?
C10 N5 N6 102.4(3) . . ?
C9 N6 N5 108.7(4) . . ?
C9 N6 Os1 115.3(3) . . ?
N5 N6 Os1 135.8(3) . . ?
C9 N7 C10 100.3(4) . . ?
C11 N8 Os1 115.0(3) . . ?
C15 N8 C11 117.4(4) . . ?
C15 N8 Os1 127.6(3) . . ?
C35 Os1 N2 170.61(17) . . ?
C35 Os1 N4 95.18(17) . . ?
C35 Os1 N6 91.35(17) . . ?
C35 Os1 N8 96.36(17) . . ?
C35 Os1 P1 90.33(14) . . ?
N2 Os1 N4 77.15(14) . . ?
N2 Os1 N8 90.37(14) . . ?
N2 Os1 P1 95.13(10) . . ?
N4 Os1 N8 165.07(13) . . ?
N4 Os1 P1 90.66(10) . . ?
N6 Os1 N2 83.74(14) . . ?
N6 Os1 N4 93.04(14) . . ?
N6 Os1 N8 77.27(13) . . ?
N6 Os1 P1 175.78(10) . . ?
N8 Os1 P1 98.69(10) . . ?
C17 P1 Os1 115.51(14) . . ?
C23 P1 C17 105.7(2) . . ?
C23 P1 Os1 113.03(15) . . ?
C29 P1 C17 103.2(2) . . ?
C29 P1 C23 101.3(2) . . ?
C29 P1 Os1 116.52(16) . . ?

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1484946'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H13 F6 N9 O Os'
_chemical_formula_sum            'C22 H13 F6 N9 O Os'
_chemical_formula_weight         723.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '
_symmetry_space_group_name_Hall  '-P1   '

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

_cell_length_a                   11.3688(8)
_cell_length_b                   11.6384(8)
_cell_length_c                   13.3026(9)
_cell_angle_alpha                68.593(2)
_cell_angle_beta                 69.189(2)
_cell_angle_gamma                84.135(2)
_cell_volume                     1531.02(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3973
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      24.27

_exptl_crystal_description       plate
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             692
_exptl_absorpt_coefficient_mu    4.230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5764
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal monochromator'
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14167
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         25.48
_reflns_number_total             5466
_reflns_number_gt                4173
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0339P)²+2.2681P] 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         5466
_refine_ls_number_parameters     650
_refine_ls_number_restraints     1377
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0877
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      0.947
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N4B N 0.3138(4) 0.0886(4) 0.1430(4) 0.0298(12) Uani 1 1 d D . .
C3B C 0.1978(5) 0.1374(5) 0.1567(6) 0.0343(16) Uani 1 1 d D A .
C4B C 0.0970(6) 0.0709(6) 0.1690(7) 0.0471(19) Uani 1 1 d D . .
H4DA H 0.0165 0.1063 0.1787 0.057 Uiso 1 1 calc R A .
C5B C 0.1138(6) -0.0472(6) 0.1671(7) 0.051(2) Uani 1 1 d D A .
H5DA H 0.0451 -0.0945 0.1758 0.061 Uiso 1 1 calc R . .
C6B C 0.2318(6) -0.0956(6) 0.1524(6) 0.0433(18) Uani 1 1 d D . .
H6DA H 0.2452 -0.1769 0.1508 0.052 Uiso 1 1 calc R A .
C7B C 0.3303(6) -0.0260(5) 0.1400(6) 0.0364(16) Uani 1 1 d D A .
H7DA H 0.4116 -0.0598 0.1291 0.044 Uiso 1 1 calc R . .
Os1 Os 0.4594(12) 0.1938(12) 0.1417(10) 0.0262(10) Uani 0.386(11) 1 d PDU A 1
N4A N 0.589(2) 0.300(2) 0.147(3) 0.037(3) Uani 0.386(11) 1 d PDU A 1
C3A C 0.695(2) 0.2398(16) 0.161(2) 0.038(3) Uani 0.386(11) 1 d PDU A 1
C4A C 0.779(2) 0.2922(16) 0.1852(18) 0.039(3) Uani 0.386(11) 1 d PDU A 1
H4AA H 0.8515 0.2490 0.1968 0.047 Uiso 0.386(11) 1 calc PR A 1
C5A C 0.7581(19) 0.4083(17) 0.1921(19) 0.041(3) Uani 0.386(11) 1 d PDU A 1
H5AA H 0.8181 0.4471 0.2051 0.049 Uiso 0.386(11) 1 calc PR A 1
C6A C 0.6498(19) 0.4682(18) 0.180(2) 0.042(3) Uani 0.386(11) 1 d PDU A 1
H6AA H 0.6330 0.5472 0.1870 0.050 Uiso 0.386(11) 1 calc PR A 1
C7A C 0.568(2) 0.4112(19) 0.158(2) 0.040(3) Uani 0.386(11) 1 d PDU A 1
H7AA H 0.4925 0.4515 0.1505 0.048 Uiso 0.386(11) 1 calc PR A 1
C1A C 0.701(2) 0.1188(17) 0.152(3) 0.034(3) Uani 0.386(11) 1 d PDU A 1
N3A N 0.786(2) 0.0300(17) 0.165(2) 0.033(3) Uani 0.386(11) 1 d PDU A 1
C2A C 0.730(2) -0.0615(16) 0.156(2) 0.032(3) Uani 0.386(11) 1 d PDU A 1
N1A N 0.620(4) -0.036(3) 0.140(6) 0.032(3) Uani 0.386(11) 1 d PDU A 1
N2A N 0.603(4) 0.082(3) 0.137(6) 0.030(3) Uani 0.386(11) 1 d PDU A 1
C8A C 0.7845(18) -0.1869(16) 0.1753(17) 0.040(3) Uani 0.386(11) 1 d PDU A 1
F1A F 0.9027(17) -0.1845(18) 0.1070(17) 0.056(5) Uani 0.386(11) 1 d PDU A 1
F2A F 0.7195(18) -0.2632(17) 0.1605(18) 0.055(4) Uani 0.386(11) 1 d PDU A 1
F3A F 0.785(2) -0.242(2) 0.2816(15) 0.070(5) Uani 0.386(11) 1 d PDU A 1
C1B C 0.189(4) 0.2609(15) 0.162(3) 0.041(6) Uani 0.386(11) 1 d PDU A 1
N3B N 0.097(3) 0.342(2) 0.179(3) 0.049(5) Uani 0.386(11) 1 d PDU A 1
C2B C 0.1617(19) 0.4337(16) 0.176(2) 0.051(4) Uani 0.386(11) 1 d PDU A 1
N1B N 0.284(2) 0.416(3) 0.160(4) 0.046(5) Uani 0.386(11) 1 d PDU A 1
N2B N 0.300(4) 0.304(3) 0.147(6) 0.040(5) Uani 0.386(11) 1 d PDU A 1
C8B C 0.1015(16) 0.5500(15) 0.1901(16) 0.069(5) Uani 0.386(11) 1 d PDU A 1
F1B F 0.1716(19) 0.6499(18) 0.1103(18) 0.100(8) Uani 0.386(11) 1 d PDU A 1
F2B F -0.0096(15) 0.5647(16) 0.178(3) 0.101(6) Uani 0.386(11) 1 d PDU A 1
F3B F 0.086(2) 0.5544(16) 0.2919(14) 0.131(7) Uani 0.386(11) 1 d PDU A 1
C14 C 0.508(6) 0.255(6) -0.0117(16) 0.036(4) Uani 0.386(11) 1 d PDU A 1
O1 O 0.535(5) 0.294(5) -0.1125(15) 0.042(5) Uani 0.386(11) 1 d PDU A 1
N5 N 0.389(5) 0.108(3) 0.3284(14) 0.035(5) Uani 0.386(11) 1 d PDU A 1
C9 C 0.386(6) -0.013(3) 0.381(2) 0.044(5) Uani 0.386(11) 1 d PDU A 1
H9A H 0.4165 -0.0651 0.3374 0.053 Uiso 0.386(11) 1 calc PR A 1
C10 C 0.338(4) -0.063(2) 0.499(2) 0.054(5) Uani 0.386(11) 1 d PDU A 1
H10A H 0.3302 -0.1504 0.5350 0.065 Uiso 0.386(11) 1 calc PR A 1
C11 C 0.303(4) 0.0073(19) 0.563(2) 0.070(6) Uani 0.386(11) 1 d PDU A 1
H11A H 0.2723 -0.0286 0.6448 0.084 Uiso 0.386(11) 1 calc PR A 1
C12 C 0.313(3) 0.129(2) 0.5105(19) 0.063(6) Uani 0.386(11) 1 d PDU A 1
H12A H 0.2908 0.1826 0.5537 0.075 Uiso 0.386(11) 1 calc PR A 1
C13 C 0.355(4) 0.176(2) 0.3943(19) 0.051(5) Uani 0.386(11) 1 d PDU A 1
H13A H 0.3612 0.2636 0.3577 0.061 Uiso 0.386(11) 1 calc PR A 1
Os1' Os 0.4546(7) 0.2028(7) 0.1235(6) 0.0263(7) Uani 0.614(11) 1 d PDU A 2
N4C N 0.5946(16) 0.3065(13) 0.1288(18) 0.038(3) Uani 0.614(11) 1 d PDU A 2
C3C C 0.7037(15) 0.2496(11) 0.1361(14) 0.039(2) Uani 0.614(11) 1 d PDU A 2
C4C C 0.8017(14) 0.3086(11) 0.1371(12) 0.046(3) Uani 0.614(11) 1 d PDU A 2
H4CA H 0.8772 0.2669 0.1411 0.056 Uiso 0.614(11) 1 calc PR A 2
C5C C 0.7884(12) 0.4291(11) 0.1321(13) 0.048(3) Uani 0.614(11) 1 d PDU A 2
H5CA H 0.8538 0.4713 0.1348 0.058 Uiso 0.614(11) 1 calc PR A 2
C6C C 0.6789(12) 0.4883(12) 0.1229(13) 0.048(3) Uani 0.614(11) 1 d PDU A 2
H6CA H 0.6685 0.5716 0.1193 0.058 Uiso 0.614(11) 1 calc PR A 2
C7C C 0.5858(13) 0.4267(12) 0.1191(13) 0.041(3) Uani 0.614(11) 1 d PDU A 2
H7CA H 0.5126 0.4693 0.1093 0.049 Uiso 0.614(11) 1 calc PR A 2
C1C C 0.7047(16) 0.1230(12) 0.1402(17) 0.033(2) Uani 0.614(11) 1 d PDU A 2
N3C N 0.7975(14) 0.0409(11) 0.1447(15) 0.032(2) Uani 0.614(11) 1 d PDU A 2
C2C C 0.7411(14) -0.0552(11) 0.1436(16) 0.032(2) Uani 0.614(11) 1 d PDU A 2
N1C N 0.625(2) -0.0393(18) 0.140(4) 0.032(2) Uani 0.614(11) 1 d PDU A 2
N2C N 0.603(2) 0.0786(18) 0.137(4) 0.030(2) Uani 0.614(11) 1 d PDU A 2
C8C C 0.8080(12) -0.1736(11) 0.1473(11) 0.035(2) Uani 0.614(11) 1 d PDU A 2
F1C F 0.9255(10) -0.1547(11) 0.0718(10) 0.047(3) Uani 0.614(11) 1 d PDU A 2
F2C F 0.7522(11) -0.2436(11) 0.1177(10) 0.051(3) Uani 0.614(11) 1 d PDU A 2
F3C F 0.8216(12) -0.2345(13) 0.2471(9) 0.060(3) Uani 0.614(11) 1 d PDU A 2
C1D C 0.198(2) 0.2623(10) 0.1553(17) 0.039(4) Uani 0.614(11) 1 d PDU A 2
N3D N 0.101(2) 0.3383(13) 0.163(2) 0.048(3) Uani 0.614(11) 1 d PDU A 2
C2D C 0.1562(13) 0.4384(12) 0.1560(14) 0.059(4) Uani 0.614(11) 1 d PDU A 2
N1D N 0.2779(15) 0.4313(17) 0.145(3) 0.051(4) Uani 0.614(11) 1 d PDU A 2
N2D N 0.303(2) 0.314(2) 0.145(4) 0.038(3) Uani 0.614(11) 1 d PDU A 2
C8D C 0.0852(11) 0.5535(11) 0.1621(12) 0.072(4) Uani 0.614(11) 1 d PDU A 2
F1D F 0.1612(12) 0.6437(12) 0.1462(14) 0.098(5) Uani 0.614(11) 1 d PDU A 2
F2D F 0.0301(9) 0.5963(8) 0.0844(10) 0.079(3) Uani 0.614(11) 1 d PDU A 2
F3D F -0.0025(11) 0.5325(9) 0.2655(9) 0.088(4) Uani 0.614(11) 1 d PDU A 2
C14' C 0.509(3) 0.263(3) -0.0320(11) 0.027(3) Uani 0.614(11) 1 d PDU A 2
O1' O 0.547(3) 0.303(3) -0.1333(9) 0.042(3) Uani 0.614(11) 1 d PDU A 2
N5' N 0.395(3) 0.1392(15) 0.3109(10) 0.035(4) Uani 0.614(11) 1 d PDU A 2
C9' C 0.387(4) 0.0202(16) 0.3735(15) 0.049(4) Uani 0.614(11) 1 d PDU A 2
H9'A H 0.4071 -0.0391 0.3367 0.058 Uiso 0.614(11) 1 calc PR A 2
C10' C 0.349(3) -0.0183(15) 0.4912(16) 0.075(5) Uani 0.614(11) 1 d PDU A 2
H10B H 0.3526 -0.1032 0.5346 0.090 Uiso 0.614(11) 1 calc PR A 2
C11' C 0.308(2) 0.0625(15) 0.5449(14) 0.074(5) Uani 0.614(11) 1 d PDU A 2
H11B H 0.2708 0.0349 0.6262 0.089 Uiso 0.614(11) 1 calc PR A 2
C12' C 0.321(2) 0.1830(16) 0.4823(14) 0.071(4) Uani 0.614(11) 1 d PDU A 2
H12B H 0.3027 0.2426 0.5187 0.085 Uiso 0.614(11) 1 calc PR A 2
C13' C 0.361(3) 0.2189(15) 0.3662(13) 0.050(4) Uani 0.614(11) 1 d PDU A 2
H13B H 0.3647 0.3046 0.3224 0.060 Uiso 0.614(11) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N4B C7B 1.341(7) . ?
N4B C3B 1.360(7) . ?
N4B Os1' 2.070(9) . ?
N4B Os1 2.149(13) . ?
C3B C4B 1.376(8) . ?
C3B C1D 1.447(10) . ?
C3B C1B 1.455(13) . ?
C4B C5B 1.377(8) . ?
C4B H4DA 0.9500 . ?
C5B C6B 1.376(8) . ?
C5B H5DA 0.9500 . ?
C6B C7B 1.377(8) . ?
C6B H6DA 0.9500 . ?
C7B H7DA 0.9500 . ?
Os1 C14 1.788(14) . ?
Os1 N2A 1.98(3) . ?
Os1 N4A 2.05(3) . ?
Os1 N2B 2.11(3) . ?
Os1 N5 2.178(14) . ?
N4A C7A 1.347(13) . ?
N4A C3A 1.365(12) . ?
C3A C4A 1.368(13) . ?
C3A C1A 1.451(11) . ?
C4A C5A 1.379(13) . ?
C4A H4AA 0.9500 . ?
C5A C6A 1.383(14) . ?
C5A H5AA 0.9500 . ?
C6A C7A 1.366(13) . ?
C6A H6AA 0.9500 . ?
C7A H7AA 0.9500 . ?
C1A N2A 1.342(12) . ?
C1A N3A 1.345(12) . ?
N3A C2A 1.355(12) . ?
C2A N1A 1.333(12) . ?
C2A C8A 1.493(12) . ?
N1A N2A 1.355(12) . ?
C8A F2A 1.319(11) . ?
C8A F1A 1.325(11) . ?
C8A F3A 1.326(12) . ?
C1B N2B 1.334(13) . ?
C1B N3B 1.344(13) . ?
N3B C2B 1.338(13) . ?
C2B N1B 1.337(13) . ?
C2B C8B 1.498(15) . ?
N1B N2B 1.362(13) . ?
C8B F2B 1.314(12) . ?
C8B F3B 1.321(12) . ?
C8B F1B 1.342(12) . ?
C14 O1 1.179(11) . ?
N5 C9 1.322(13) . ?
N5 C13 1.323(13) . ?
C9 C10 1.369(15) . ?
C9 H9A 0.9500 . ?
C10 C11 1.332(15) . ?
C10 H10A 0.9500 . ?
C11 C12 1.332(15) . ?
C11 H11A 0.9500 . ?
C12 C13 1.352(15) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
Os1' C14' 1.810(11) . ?
Os1' N2D 2.046(16) . ?
Os1' N2C 2.120(16) . ?
Os1' N4C 2.127(18) . ?
Os1' N5' 2.186(11) . ?
N4C C7C 1.353(10) . ?
N4C C3C 1.363(10) . ?
C3C C4C 1.373(11) . ?
C3C C1C 1.453(9) . ?
C4C C5C 1.375(11) . ?
C4C H4CA 0.9500 . ?
C5C C6C 1.383(11) . ?
C5C H5CA 0.9500 . ?
C6C C7C 1.362(11) . ?
C6C H6CA 0.9500 . ?
C7C H7CA 0.9500 . ?
C1C N2C 1.335(10) . ?
C1C N3C 1.351(10) . ?
N3C C2C 1.352(9) . ?
C2C N1C 1.329(10) . ?
C2C C8C 1.498(10) . ?
N1C N2C 1.358(9) . ?
C8C F3C 1.313(9) . ?
C8C F2C 1.318(9) . ?
C8C F1C 1.336(9) . ?
C1D N2D 1.332(10) . ?
C1D N3D 1.340(10) . ?
N3D C2D 1.338(11) . ?
C2D N1D 1.335(11) . ?
C2D C8D 1.505(13) . ?
N1D N2D 1.367(10) . ?
C8D F2D 1.316(11) . ?
C8D F3D 1.333(11) . ?
C8D F1D 1.336(11) . ?
C14' O1' 1.178(10) . ?
N5' C9' 1.323(11) . ?
N5' C13' 1.332(11) . ?
C9' C10' 1.373(13) . ?
C9' H9'A 0.9500 . ?
C10' C11' 1.334(13) . ?
C10' H10B 0.9500 . ?
C11' C12' 1.336(13) . ?
C11' H11B 0.9500 . ?
C12' C13' 1.355(13) . ?
C12' H12B 0.9500 . ?
C13' H13B 0.9500 . ?

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
C7B N4B C3B 119.1(5) . . ?
C7B N4B Os1' 124.9(4) . . ?
C3B N4B Os1' 115.9(4) . . ?
C7B N4B Os1 122.7(5) . . ?
C3B N4B Os1 117.9(5) . . ?
Os1' N4B Os1 6.4(4) . . ?
N4B C3B C4B 121.3(5) . . ?
N4B C3B C1D 111.6(11) . . ?
C4B C3B C1D 127.1(12) . . ?
N4B C3B C1B 115.1(18) . . ?
C4B C3B C1B 123.6(18) . . ?
C1D C3B C1B 4(2) . . ?
C3B C4B C5B 119.5(6) . . ?
C3B C4B H4DA 120.2 . . ?
C5B C4B H4DA 120.2 . . ?
C6B C5B C4B 118.8(6) . . ?
C6B C5B H5DA 120.6 . . ?
C4B C5B H5DA 120.6 . . ?
C5B C6B C7B 119.9(6) . . ?
C5B C6B H6DA 120.0 . . ?
C7B C6B H6DA 120.0 . . ?
N4B C7B C6B 121.3(6) . . ?
N4B C7B H7DA 119.3 . . ?
C6B C7B H7DA 119.3 . . ?
C14 Os1 N2A 92(3) . . ?
C14 Os1 N4A 94(2) . . ?
N2A Os1 N4A 79.5(11) . . ?
C14 Os1 N2B 88(3) . . ?
N2A Os1 N2B 176.3(15) . . ?
N4A Os1 N2B 104.2(14) . . ?
C14 Os1 N4B 88(2) . . ?
N2A Os1 N4B 103.8(9) . . ?
N4A Os1 N4B 176.1(10) . . ?
N2B Os1 N4B 72.5(12) . . ?
C14 Os1 N5 175(2) . . ?
N2A Os1 N5 89(2) . . ?
N4A Os1 N5 91.4(16) . . ?
N2B Os1 N5 91(2) . . ?
N4B Os1 N5 86.7(14) . . ?
C7A N4A C3A 119.0(14) . . ?
C7A N4A Os1 125.1(14) . . ?
C3A N4A Os1 114.7(12) . . ?
N4A C3A C4A 121.0(12) . . ?
N4A C3A C1A 112.4(10) . . ?
C4A C3A C1A 126.6(11) . . ?
C3A C4A C5A 119.3(13) . . ?
C3A C4A H4AA 120.4 . . ?
C5A C4A H4AA 120.4 . . ?
C4A C5A C6A 120.0(13) . . ?
C4A C5A H5AA 120.0 . . ?
C6A C5A H5AA 120.0 . . ?
C7A C6A C5A 118.4(13) . . ?
C7A C6A H6AA 120.8 . . ?
C5A C6A H6AA 120.8 . . ?
N4A C7A C6A 122.4(15) . . ?
N4A C7A H7AA 118.8 . . ?
C6A C7A H7AA 118.8 . . ?
N2A C1A N3A 112.1(11) . . ?
N2A C1A C3A 116.7(11) . . ?
N3A C1A C3A 130.9(11) . . ?
C1A N3A C2A 100.4(11) . . ?
N1A C2A N3A 116.3(11) . . ?
N1A C2A C8A 122.4(10) . . ?
N3A C2A C8A 121.0(10) . . ?
C2A N1A N2A 102.5(12) . . ?
C1A N2A N1A 108.7(12) . . ?
C1A N2A Os1 115.7(14) . . ?
N1A N2A Os1 134.6(14) . . ?
F2A C8A F1A 107.6(11) . . ?
F2A C8A F3A 105.1(11) . . ?
F1A C8A F3A 105.8(11) . . ?
F2A C8A C2A 112.7(10) . . ?
F1A C8A C2A 112.9(10) . . ?
F3A C8A C2A 112.2(10) . . ?
N2B C1B N3B 112.0(12) . . ?
N2B C1B C3B 111(3) . . ?
N3B C1B C3B 137(3) . . ?
C2B N3B C1B 100.9(11) . . ?
N1B C2B N3B 116.4(12) . . ?
N1B C2B C8B 121.1(11) . . ?
N3B C2B C8B 122.5(11) . . ?
C2B N1B N2B 102.1(12) . . ?
C1B N2B N1B 108.5(13) . . ?
C1B N2B Os1 123(2) . . ?
N1B N2B Os1 128(2) . . ?
F2B C8B F3B 107.2(12) . . ?
F2B C8B F1B 105.7(12) . . ?
F3B C8B F1B 107.3(12) . . ?
F2B C8B C2B 112.9(11) . . ?
F3B C8B C2B 112.3(11) . . ?
F1B C8B C2B 111.1(11) . . ?
O1 C14 Os1 178(5) . . ?
C9 N5 C13 116.8(16) . . ?
C9 N5 Os1 122.2(17) . . ?
C13 N5 Os1 120.9(17) . . ?
N5 C9 C10 120.4(16) . . ?
N5 C9 H9A 119.8 . . ?
C10 C9 H9A 119.8 . . ?
C11 C10 C9 121.6(17) . . ?
C11 C10 H10A 119.2 . . ?
C9 C10 H10A 119.2 . . ?
C12 C11 C10 118.2(19) . . ?
C12 C11 H11A 120.9 . . ?
C10 C11 H11A 120.9 . . ?
C11 C12 C13 118.9(18) . . ?
C11 C12 H12A 120.6 . . ?
C13 C12 H12A 120.6 . . ?
N5 C13 C12 124.0(16) . . ?
N5 C13 H13A 118.0 . . ?
C12 C13 H13A 118.0 . . ?
C14' Os1' N2D 95.5(17) . . ?
C14' Os1' N4B 95.4(12) . . ?
N2D Os1' N4B 79.1(8) . . ?
C14' Os1' N2C 95.7(17) . . ?
N2D Os1' N2C 168.6(18) . . ?
N4B Os1' N2C 101.7(6) . . ?
C14' Os1' N4C 92.6(13) . . ?
N2D Os1' N4C 101.8(9) . . ?
N4B Os1' N4C 171.8(7) . . ?
N2C Os1' N4C 75.8(6) . . ?
C14' Os1' N5' 176.6(14) . . ?
N2D Os1' N5' 84.1(14) . . ?
N4B Os1' N5' 87.9(8) . . ?
N2C Os1' N5' 84.6(15) . . ?
N4C Os1' N5' 84.2(10) . . ?
C7C N4C C3C 117.7(10) . . ?
C7C N4C Os1' 124.7(9) . . ?
C3C N4C Os1' 117.5(8) . . ?
N4C C3C C4C 122.5(9) . . ?
N4C C3C C1C 112.8(8) . . ?
C4C C3C C1C 124.7(8) . . ?
C3C C4C C5C 118.6(10) . . ?
C3C C4C H4CA 120.7 . . ?
C5C C4C H4CA 120.7 . . ?
C4C C5C C6C 119.4(10) . . ?
C4C C5C H5CA 120.3 . . ?
C6C C5C H5CA 120.3 . . ?
C7C C6C C5C 119.7(10) . . ?
C7C C6C H6CA 120.2 . . ?
C5C C6C H6CA 120.2 . . ?
N4C C7C C6C 122.0(10) . . ?
N4C C7C H7CA 119.0 . . ?
C6C C7C H7CA 119.0 . . ?
N2C C1C N3C 113.1(8) . . ?
N2C C1C C3C 117.9(8) . . ?
N3C C1C C3C 128.9(8) . . ?
C1C N3C C2C 99.3(8) . . ?
N1C C2C N3C 116.9(8) . . ?
N1C C2C C8C 122.5(8) . . ?
N3C C2C C8C 120.5(8) . . ?
C2C N1C N2C 102.6(8) . . ?
C1C N2C N1C 107.9(9) . . ?
C1C N2C Os1' 116.0(8) . . ?
N1C N2C Os1' 136.0(8) . . ?
F3C C8C F2C 111.1(8) . . ?
F3C C8C F1C 104.4(8) . . ?
F2C C8C F1C 104.8(8) . . ?
F3C C8C C2C 112.9(8) . . ?
F2C C8C C2C 111.1(8) . . ?
F1C C8C C2C 112.1(8) . . ?
N2D C1D N3D 112.6(9) . . ?
N2D C1D C3B 120.3(17) . . ?
N3D C1D C3B 127.1(16) . . ?
C2D N3D C1D 100.5(8) . . ?
N1D C2D N3D 116.8(9) . . ?
N1D C2D C8D 121.0(9) . . ?
N3D C2D C8D 122.2(9) . . ?
C2D N1D N2D 101.8(9) . . ?
C1D N2D N1D 108.3(9) . . ?
C1D N2D Os1' 113.0(14) . . ?
N1D N2D Os1' 138.5(13) . . ?
F2D C8D F3D 108.3(10) . . ?
F2D C8D F1D 107.5(10) . . ?
F3D C8D F1D 106.2(10) . . ?
F2D C8D C2D 112.2(10) . . ?
F3D C8D C2D 110.9(9) . . ?
F1D C8D C2D 111.5(9) . . ?
O1' C14' Os1' 179(3) . . ?
C9' N5' C13' 117.7(11) . . ?
C9' N5' Os1' 121.2(12) . . ?
C13' N5' Os1' 121.0(10) . . ?
N5' C9' C10' 120.5(13) . . ?
N5' C9' H9'A 119.7 . . ?
C10' C9' H9'A 119.7 . . ?
C11' C10' C9' 120.5(14) . . ?
C11' C10' H10B 119.7 . . ?
C9' C10' H10B 119.7 . . ?
C10' C11' C12' 118.8(15) . . ?
C10' C11' H11B 120.6 . . ?
C12' C11' H11B 120.6 . . ?
C11' C12' C13' 119.0(14) . . ?
C11' C12' H12B 120.5 . . ?
C13' C12' H12B 120.5 . . ?
N5' C13' C12' 122.8(12) . . ?
N5' C13' H13B 118.6 . . ?
C12' C13' H13B 118.6 . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.003 -0.034 0.500 426 78 ' '
_platon_squeeze_details          
;
;

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        25.48
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.141
