# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H15 F6 N5 O5 Os'
_chemical_formula_weight         697.56

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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   9.4606(8)
_cell_length_b                   19.8658(17)
_cell_length_c                   12.5770(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.686(2)
_cell_angle_gamma                90.00
_cell_volume                     2252.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7495
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.50

_exptl_crystal_description       plate
_exptl_crystal_colour            light-yellow
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    5.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2184
_exptl_absorpt_correction_T_max  0.8463
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16159
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5177
_reflns_number_gt                4693
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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     
'calc w=1/[σ²(Fo²)+(0.0325P)²+1.2564P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5177
_refine_ls_number_parameters     335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_ref         0.0808
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 1.045204(14) 0.511417(8) 0.714157(11) 0.01458(7) Uani 1 1 d . . .
O1 O 1.2891(3) 0.54678(17) 0.6129(2) 0.0254(7) Uani 1 1 d . . .
O2 O 1.1126(3) 0.64344(17) 0.8342(2) 0.0308(7) Uani 1 1 d . . .
O3 O 0.9847(3) 0.41999(18) 0.6216(3) 0.0199(6) Uani 1 1 d . . .
H3A H 1.034(6) 0.417(3) 0.580(5) 0.050(18) Uiso 1 1 d . . .
H3B H 0.975(6) 0.388(3) 0.646(4) 0.031(17) Uiso 1 1 d . . .
N1 N 1.2961(3) 0.43805(18) 0.9049(3) 0.0179(7) Uani 1 1 d . . .
N2 N 1.1536(3) 0.45425(17) 0.8540(3) 0.0162(7) Uani 1 1 d . . .
N3 N 0.8755(4) 0.48481(17) 0.7774(3) 0.0170(7) Uani 1 1 d . . .
N4 N 0.8599(3) 0.55244(17) 0.5983(3) 0.0165(7) Uani 1 1 d . . .
N5 N 0.8389(3) 0.59321(17) 0.5087(3) 0.0179(7) Uani 1 1 d . . .
C1 C 1.1975(4) 0.5320(2) 0.6496(3) 0.0190(8) Uani 1 1 d . . .
C2 C 1.0879(4) 0.5924(2) 0.7900(3) 0.0194(8) Uani 1 1 d . . .
C3 C 1.4354(4) 0.3752(2) 1.0703(3) 0.0232(9) Uani 1 1 d . . .
C4 C 1.2936(4) 0.4030(2) 0.9958(3) 0.0194(8) Uani 1 1 d . . .
C5 C 1.1517(4) 0.3968(2) 1.0059(3) 0.0184(8) Uani 1 1 d . . .
H5 H 1.1222 0.3748 1.0627 0.022 Uiso 1 1 calc R . .
C6 C 1.0647(4) 0.4303(2) 0.9137(3) 0.0168(8) Uani 1 1 d . . .
C7 C 0.9060(4) 0.4461(2) 0.8699(3) 0.0165(8) Uani 1 1 d . . .
C8 C 0.7930(4) 0.4269(2) 0.9118(3) 0.0205(8) Uani 1 1 d . . .
H8 H 0.8129 0.3999 0.9771 0.025 Uiso 1 1 calc R . .
C9 C 0.6495(4) 0.4480(2) 0.8561(3) 0.0226(9) Uani 1 1 d . . .
H9 H 0.5707 0.4358 0.8844 0.027 Uiso 1 1 calc R . .
C10 C 0.6198(4) 0.4862(2) 0.7604(4) 0.0219(9) Uani 1 1 d . . .
H10 H 0.5212 0.4999 0.7220 0.026 Uiso 1 1 calc R . .
C11 C 0.7366(4) 0.5043(2) 0.7212(4) 0.0177(8) Uani 1 1 d . . .
C12 C 0.7300(4) 0.5451(2) 0.6230(3) 0.0184(8) Uani 1 1 d . . .
C13 C 0.6212(4) 0.5821(2) 0.5470(3) 0.0216(9) Uani 1 1 d . . .
H13 H 0.5197 0.5868 0.5429 0.026 Uiso 1 1 calc R . .
C14 C 0.6939(4) 0.6104(2) 0.4793(3) 0.0204(8) Uani 1 1 d . . .
C15 C 0.6346(4) 0.6572(2) 0.3836(3) 0.0249(9) Uani 1 1 d . . .
F1 F 1.5457(3) 0.42063(15) 1.0965(2) 0.0346(7) Uani 1 1 d . . .
F2 F 1.4198(3) 0.35312(15) 1.1668(2) 0.0348(7) Uani 1 1 d . . .
F3 F 1.4857(3) 0.32279(16) 1.0251(2) 0.0419(7) Uani 1 1 d . . .
F4 F 0.4931(3) 0.67149(18) 0.3687(2) 0.0467(8) Uani 1 1 d . . .
F5 F 0.6444(3) 0.63163(15) 0.2872(2) 0.0365(7) Uani 1 1 d . . .
F6 F 0.7096(3) 0.71508(15) 0.3970(2) 0.0426(7) Uani 1 1 d . . .
O4 O 0.9066(4) 0.31424(18) 0.7242(3) 0.0370(8) Uani 1 1 d . . .
O5 O 0.9120(3) 0.24014(17) 0.8577(2) 0.0307(7) Uani 1 1 d . . .
C16 C 0.9747(5) 0.2742(3) 0.7935(3) 0.0312(11) Uani 1 1 d . . .
C17 C 1.1350(5) 0.2576(3) 0.8165(5) 0.0453(13) Uani 1 1 d . . .
H17A H 1.1484 0.2313 0.7544 0.068 Uiso 1 1 calc R . .
H17B H 1.1693 0.2313 0.8855 0.068 Uiso 1 1 calc R . .
H17C H 1.1925 0.2993 0.8247 0.068 Uiso 1 1 calc R . .
C18 C 0.7531(5) 0.2485(3) 0.8362(4) 0.0364(11) Uani 1 1 d . . .
H18A H 0.6981 0.2231 0.7685 0.044 Uiso 1 1 calc R . .
H18B H 0.7258 0.2966 0.8243 0.044 Uiso 1 1 calc R . .
C19 C 0.7150(7) 0.2220(3) 0.9365(5) 0.0532(15) Uani 1 1 d . . .
H19A H 0.7437 0.1745 0.9480 0.080 Uiso 1 1 calc R . .
H19B H 0.6080 0.2263 0.9240 0.080 Uiso 1 1 calc R . .
H19C H 0.7686 0.2480 1.0027 0.080 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os C2 1.851(4) . ?
Os C1 1.901(4) . ?
Os N3 2.065(3) . ?
Os N4 2.076(3) . ?
Os N2 2.083(3) . ?
Os O3 2.139(3) . ?
O1 C1 1.137(5) . ?
O2 C2 1.146(5) . ?
N1 N2 1.344(4) . ?
N1 C4 1.345(5) . ?
N2 C6 1.372(5) . ?
N3 C11 1.347(5) . ?
N3 C7 1.350(5) . ?
N4 N5 1.352(4) . ?
N4 C12 1.364(5) . ?
N5 C14 1.351(5) . ?
C3 F3 1.340(5) . ?
C3 F2 1.340(5) . ?
C3 F1 1.343(5) . ?
C3 C4 1.490(5) . ?
C4 C5 1.391(5) . ?
C5 C6 1.373(5) . ?
C6 C7 1.468(5) . ?
C7 C8 1.381(5) . ?
C8 C9 1.390(5) . ?
C9 C10 1.378(6) . ?
C10 C11 1.387(6) . ?
C11 C12 1.463(6) . ?
C12 C13 1.384(5) . ?
C13 C14 1.368(6) . ?
C14 C15 1.488(6) . ?
C15 F4 1.325(5) . ?
C15 F6 1.336(5) . ?
C15 F5 1.344(5) . ?
O4 C16 1.212(6) . ?
O5 C16 1.324(5) . ?
O5 C18 1.454(5) . ?
C16 C17 1.491(7) . ?
C18 C19 1.508(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Os C1 87.61(18) . . ?
C2 Os N3 95.59(15) . . ?
C1 Os N3 176.69(15) . . ?
C2 Os N4 91.48(15) . . ?
C1 Os N4 101.77(14) . . ?
N3 Os N4 77.37(13) . . ?
C2 Os N2 93.71(14) . . ?
C1 Os N2 103.59(14) . . ?
N3 Os N2 77.07(13) . . ?
N4 Os N2 154.29(12) . . ?
C2 Os O3 176.95(13) . . ?
C1 Os O3 93.57(16) . . ?
N3 Os O3 83.19(13) . . ?
N4 Os O3 85.53(13) . . ?
N2 Os O3 88.75(12) . . ?
N2 N1 C4 104.7(3) . . ?
N1 N2 C6 110.5(3) . . ?
N1 N2 Os 134.3(3) . . ?
C6 N2 Os 115.1(2) . . ?
C11 N3 C7 122.3(4) . . ?
C11 N3 Os 118.3(3) . . ?
C7 N3 Os 119.4(3) . . ?
N5 N4 C12 109.8(3) . . ?
N5 N4 Os 134.4(2) . . ?
C12 N4 Os 115.2(2) . . ?
C14 N5 N4 105.1(3) . . ?
O1 C1 Os 177.2(4) . . ?
O2 C2 Os 178.1(4) . . ?
F3 C3 F2 106.3(4) . . ?
F3 C3 F1 106.1(3) . . ?
F2 C3 F1 106.8(3) . . ?
F3 C3 C4 112.9(3) . . ?
F2 C3 C4 111.4(3) . . ?
F1 C3 C4 112.9(4) . . ?
N1 C4 C5 112.9(3) . . ?
N1 C4 C3 118.8(3) . . ?
C5 C4 C3 128.3(4) . . ?
C6 C5 C4 103.2(3) . . ?
N2 C6 C5 108.7(3) . . ?
N2 C6 C7 116.6(3) . . ?
C5 C6 C7 134.7(4) . . ?
N3 C7 C8 119.9(3) . . ?
N3 C7 C6 111.8(3) . . ?
C8 C7 C6 128.3(4) . . ?
C7 C8 C9 118.4(4) . . ?
C10 C9 C8 121.0(4) . . ?
C9 C10 C11 118.7(4) . . ?
N3 C11 C10 119.7(4) . . ?
N3 C11 C12 112.8(3) . . ?
C10 C11 C12 127.6(4) . . ?
N4 C12 C13 108.6(3) . . ?
N4 C12 C11 116.2(3) . . ?
C13 C12 C11 135.2(4) . . ?
C14 C13 C12 103.8(3) . . ?
N5 C14 C13 112.7(3) . . ?
N5 C14 C15 118.8(4) . . ?
C13 C14 C15 128.5(4) . . ?
F4 C15 F6 108.0(4) . . ?
F4 C15 F5 107.3(3) . . ?
F6 C15 F5 105.0(4) . . ?
F4 C15 C14 111.4(3) . . ?
F6 C15 C14 112.3(3) . . ?
F5 C15 C14 112.5(4) . . ?
C16 O5 C18 117.3(4) . . ?
O4 C16 O5 122.3(4) . . ?
O4 C16 C17 124.9(4) . . ?
O5 C16 C17 112.7(4) . . ?
O5 C18 C19 107.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.678
_refine_diff_density_min         -1.853
_refine_diff_density_rms         0.160
_database_code_depnum_ccdc_archive 'CCDC 989382'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H31 F6 N5 O Os P2'
_chemical_formula_weight         963.84

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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   20.3095(11)
_cell_length_b                   18.5039(10)
_cell_length_c                   22.1017(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.9652(11)
_cell_angle_gamma                90.00
_cell_volume                     7529.9(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8435
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      27.42

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.38
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3792
_exptl_absorpt_coefficient_mu    3.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3177
_exptl_absorpt_correction_T_max  0.3463
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48752
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.11
_diffrn_reflns_theta_max         27.50
_reflns_number_total             17269
_reflns_number_gt                15177
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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     
'calc w=1/[σ²(Fo²)+(0.0302P)²+3.6516P] 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         17269
_refine_ls_number_parameters     1014
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0684
_refine_ls_wR_factor_gt          0.0658
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.025
_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
Os1 Os 0.984615(7) 0.710975(6) 0.628449(6) 0.01441(4) Uani 1 1 d . . .
P1 P 0.94575(5) 0.66892(4) 0.51739(4) 0.01816(18) Uani 1 1 d . . .
P2 P 1.02299(5) 0.75673(4) 0.73819(4) 0.01769(17) Uani 1 1 d . . .
O1 O 1.10442(14) 0.59963(14) 0.67794(13) 0.0345(6) Uani 1 1 d . . .
N1 N 1.09656(14) 0.82092(14) 0.61333(13) 0.0179(6) Uani 1 1 d . . .
N2 N 1.02946(14) 0.80265(14) 0.60575(13) 0.0159(6) Uani 1 1 d . . .
N3 N 0.89863(14) 0.78399(14) 0.59399(13) 0.0164(6) Uani 1 1 d . . .
N4 N 0.90104(14) 0.65425(14) 0.63676(13) 0.0183(6) Uani 1 1 d . . .
N5 N 0.89675(15) 0.58890(14) 0.66104(14) 0.0209(6) Uani 1 1 d . . .
C1 C 1.05955(18) 0.64292(18) 0.65923(17) 0.0209(7) Uani 1 1 d . . .
C2 C 1.15784(18) 0.92927(18) 0.60108(17) 0.0217(7) Uani 1 1 d . . .
C3 C 1.09174(17) 0.89120(17) 0.59543(16) 0.0179(7) Uani 1 1 d . . .
C4 C 1.02267(18) 0.91902(17) 0.57634(16) 0.0202(7) Uani 1 1 d . . .
H4 H 1.0059 0.9666 0.5617 0.024 Uiso 1 1 calc R . .
C5 C 0.98374(17) 0.86051(17) 0.58374(16) 0.0180(7) Uani 1 1 d . . .
C6 C 0.90914(17) 0.85005(17) 0.57420(15) 0.0173(7) Uani 1 1 d . . .
C7 C 0.85203(19) 0.89888(18) 0.55012(17) 0.0232(7) Uani 1 1 d . . .
H7 H 0.8587 0.9456 0.5358 0.028 Uiso 1 1 calc R . .
C8 C 0.7855(2) 0.8786(2) 0.54731(19) 0.0284(8) Uani 1 1 d . . .
H8 H 0.7460 0.9115 0.5307 0.034 Uiso 1 1 calc R . .
C9 C 0.77568(18) 0.81048(19) 0.56846(18) 0.0252(8) Uani 1 1 d . . .
H9 H 0.7300 0.7968 0.5670 0.030 Uiso 1 1 calc R . .
C10 C 0.83391(18) 0.76277(18) 0.59177(16) 0.0193(7) Uani 1 1 d . . .
C11 C 0.83582(18) 0.68996(18) 0.61625(17) 0.0206(7) Uani 1 1 d . . .
C12 C 0.78766(19) 0.64557(19) 0.62787(18) 0.0249(8) Uani 1 1 d . . .
H12 H 0.7384 0.6549 0.6188 0.030 Uiso 1 1 calc R . .
C13 C 0.82825(19) 0.58442(18) 0.65582(18) 0.0235(7) Uani 1 1 d . A .
C14 C 0.8085(2) 0.5208(2) 0.6846(2) 0.0348(9) Uani 1 1 d D . .
C15 C 0.8860(2) 0.59134(19) 0.49943(18) 0.0296(9) Uani 1 1 d . . .
H15A H 0.8444 0.6032 0.5091 0.044 Uiso 1 1 calc R . .
H15B H 0.9125 0.5505 0.5272 0.044 Uiso 1 1 calc R . .
H15C H 0.8687 0.5784 0.4522 0.044 Uiso 1 1 calc R . .
C16 C 0.89396(18) 0.73596(18) 0.45508(16) 0.0200(7) Uani 1 1 d . . .
C17 C 0.81932(19) 0.74163(19) 0.43191(18) 0.0265(8) Uani 1 1 d . . .
H17 H 0.7935 0.7080 0.4462 0.032 Uiso 1 1 calc R . .
C18 C 0.7820(2) 0.7968(2) 0.38743(19) 0.0345(10) Uani 1 1 d . . .
H18 H 0.7307 0.8008 0.3715 0.041 Uiso 1 1 calc R . .
C19 C 0.8200(2) 0.8453(2) 0.36686(19) 0.0363(10) Uani 1 1 d . . .
H19 H 0.7946 0.8825 0.3363 0.044 Uiso 1 1 calc R . .
C20 C 0.8942(2) 0.8404(2) 0.39019(19) 0.0321(9) Uani 1 1 d . . .
H20 H 0.9200 0.8745 0.3763 0.039 Uiso 1 1 calc R . .
C21 C 0.9309(2) 0.78594(18) 0.43378(18) 0.0256(8) Uani 1 1 d . . .
H21 H 0.9822 0.7824 0.4495 0.031 Uiso 1 1 calc R . .
C22 C 1.01622(19) 0.64120(18) 0.49163(17) 0.0223(7) Uani 1 1 d . . .
C23 C 0.9979(2) 0.6012(2) 0.43291(18) 0.0323(9) Uani 1 1 d . . .
H23 H 0.9485 0.5899 0.4057 0.039 Uiso 1 1 calc R . .
C24 C 1.0518(2) 0.5782(2) 0.4145(2) 0.0382(10) Uani 1 1 d . . .
H24 H 1.0392 0.5505 0.3750 0.046 Uiso 1 1 calc R . .
C25 C 1.1235(2) 0.5952(2) 0.4531(2) 0.0353(10) Uani 1 1 d . . .
H25 H 1.1604 0.5786 0.4407 0.042 Uiso 1 1 calc R . .
C26 C 1.1414(2) 0.6362(2) 0.5095(2) 0.0344(9) Uani 1 1 d . . .
H26 H 1.1907 0.6488 0.5356 0.041 Uiso 1 1 calc R . .
C27 C 1.0883(2) 0.65940(19) 0.52891(19) 0.0274(8) Uani 1 1 d . . .
H27 H 1.1014 0.6880 0.5680 0.033 Uiso 1 1 calc R . .
C28 C 1.10248(19) 0.81434(19) 0.76367(18) 0.0269(8) Uani 1 1 d . . .
H28A H 1.0943 0.8515 0.7297 0.040 Uiso 1 1 calc R . .
H28B H 1.1448 0.7851 0.7688 0.040 Uiso 1 1 calc R . .
H28C H 1.1113 0.8375 0.8063 0.040 Uiso 1 1 calc R . .
C29 C 1.04832(18) 0.69330(18) 0.80766(17) 0.0197(7) Uani 1 1 d . . .
C30 C 1.0811(2) 0.71966(19) 0.87266(18) 0.0270(8) Uani 1 1 d . . .
H30 H 1.0893 0.7701 0.8802 0.032 Uiso 1 1 calc R . .
C31 C 1.1015(2) 0.67325(19) 0.92602(18) 0.0298(9) Uani 1 1 d . . .
H31 H 1.1245 0.6917 0.9702 0.036 Uiso 1 1 calc R . .
C32 C 1.0888(2) 0.6000(2) 0.91579(19) 0.0320(9) Uani 1 1 d . . .
H32 H 1.1026 0.5682 0.9528 0.038 Uiso 1 1 calc R . .
C33 C 1.0561(2) 0.57322(19) 0.85153(18) 0.0291(8) Uani 1 1 d . . .
H33 H 1.0472 0.5228 0.8443 0.035 Uiso 1 1 calc R . .
C34 C 1.03592(19) 0.62005(18) 0.79720(17) 0.0234(7) Uani 1 1 d . . .
H34 H 1.0137 0.6015 0.7530 0.028 Uiso 1 1 calc R . .
C35 C 0.95395(18) 0.81234(18) 0.74815(16) 0.0203(7) Uani 1 1 d . . .
C36 C 0.8996(2) 0.77923(19) 0.76009(18) 0.0258(8) Uani 1 1 d . . .
H36 H 0.9013 0.7286 0.7676 0.031 Uiso 1 1 calc R . .
C37 C 0.8424(2) 0.8195(2) 0.7612(2) 0.0333(9) Uani 1 1 d . . .
H37 H 0.8048 0.7965 0.7690 0.040 Uiso 1 1 calc R . .
C38 C 0.8407(2) 0.8931(2) 0.7510(2) 0.0378(10) Uani 1 1 d . . .
H38 H 0.8016 0.9208 0.7516 0.045 Uiso 1 1 calc R . .
C39 C 0.8947(2) 0.9267(2) 0.7401(2) 0.0373(10) Uani 1 1 d . . .
H39 H 0.8932 0.9776 0.7337 0.045 Uiso 1 1 calc R . .
C40 C 0.9516(2) 0.88682(19) 0.73828(18) 0.0282(8) Uani 1 1 d . . .
H40 H 0.9889 0.9102 0.7303 0.034 Uiso 1 1 calc R . .
F1 F 1.19455(11) 0.89285(11) 0.57241(10) 0.0291(5) Uani 1 1 d . . .
F2 F 1.14217(12) 0.99402(11) 0.57123(11) 0.0348(5) Uani 1 1 d . . .
F3 F 1.20565(11) 0.94091(12) 0.66415(10) 0.0320(5) Uani 1 1 d . . .
F4 F 0.8511(3) 0.5155(3) 0.7525(2) 0.0634(14) Uani 0.754(4) 1 d PDU A 1
F5 F 0.7412(2) 0.5187(3) 0.6765(2) 0.0445(11) Uani 0.754(4) 1 d PDU A 1
F6 F 0.8270(6) 0.4581(6) 0.6661(7) 0.0371(19) Uani 0.754(4) 1 d PD A 1
F4' F 0.8169(9) 0.5321(9) 0.7446(7) 0.0634(14) Uani 0.246(4) 1 d PDU A 2
F5' F 0.7289(7) 0.5189(10) 0.6487(7) 0.0445(11) Uani 0.246(4) 1 d PDU A 2
F6' F 0.813(2) 0.459(2) 0.655(3) 0.0371(19) Uani 0.246(4) 1 d PD A 2
Os2 Os 0.496693(6) 0.279229(6) 0.648444(6) 0.01495(4) Uani 1 1 d . . .
P3 P 0.51065(5) 0.16201(4) 0.61216(4) 0.01754(18) Uani 1 1 d . . .
P4 P 0.48905(5) 0.39869(4) 0.68437(4) 0.01756(17) Uani 1 1 d . . .
O2 O 0.34905(14) 0.29968(15) 0.53429(13) 0.0357(7) Uani 1 1 d . . .
N6 N 0.56439(15) 0.34497(15) 0.55534(14) 0.0206(6) Uani 1 1 d . . .
N7 N 0.57018(14) 0.31751(14) 0.61357(13) 0.0175(6) Uani 1 1 d . . .
N8 N 0.59590(14) 0.26757(14) 0.73027(13) 0.0162(6) Uani 1 1 d . A .
N9 N 0.46894(14) 0.23375(14) 0.72007(14) 0.0176(6) Uani 1 1 d . . .
N10 N 0.40638(15) 0.21079(14) 0.71962(14) 0.0197(6) Uani 1 1 d . . .
C41 C 0.40592(19) 0.29115(17) 0.57702(17) 0.0207(7) Uani 1 1 d . . .
C42 C 0.6459(2) 0.3965(2) 0.51175(19) 0.0357(10) Uani 1 1 d D . .
C43 C 0.63248(19) 0.36420(19) 0.56614(17) 0.0231(7) Uani 1 1 d . A .
C44 C 0.68273(18) 0.34924(18) 0.63013(17) 0.0208(7) Uani 1 1 d . . .
H44 H 0.7336 0.3577 0.6493 0.025 Uiso 1 1 calc R A .
C45 C 0.64119(18) 0.31900(17) 0.65962(16) 0.0185(7) Uani 1 1 d . A .
C46 C 0.65678(18) 0.29020(16) 0.72542(17) 0.0181(7) Uani 1 1 d . . .
C47 C 0.72336(18) 0.28517(17) 0.78020(18) 0.0230(7) Uani 1 1 d . A .
H47 H 0.7665 0.3007 0.7773 0.028 Uiso 1 1 calc R . .
C48 C 0.72579(19) 0.25718(19) 0.83902(18) 0.0255(8) Uani 1 1 d . . .
H48 H 0.7712 0.2531 0.8768 0.031 Uiso 1 1 calc R A .
C49 C 0.66281(18) 0.23490(18) 0.84376(17) 0.0235(7) Uani 1 1 d . A .
H49 H 0.6646 0.2163 0.8845 0.028 Uiso 1 1 calc R . .
C50 C 0.59707(17) 0.24040(17) 0.78748(16) 0.0176(7) Uani 1 1 d . . .
C51 C 0.52554(18) 0.21987(16) 0.78054(16) 0.0180(7) Uani 1 1 d . A .
C52 C 0.49776(18) 0.18679(18) 0.82138(17) 0.0207(7) Uani 1 1 d . . .
H52 H 0.5232 0.1711 0.8662 0.025 Uiso 1 1 calc R A .
C53 C 0.42410(18) 0.18230(18) 0.78087(17) 0.0206(7) Uani 1 1 d . A .
C54 C 0.3661(2) 0.15034(19) 0.79638(18) 0.0264(8) Uani 1 1 d . . .
C55 C 0.4907(2) 0.09022(19) 0.65780(18) 0.0276(8) Uani 1 1 d . . .
H55A H 0.4387 0.0902 0.6469 0.041 Uiso 1 1 calc R . .
H55B H 0.5185 0.0980 0.7058 0.041 Uiso 1 1 calc R . .
H55C H 0.5043 0.0436 0.6453 0.041 Uiso 1 1 calc R . .
C56 C 0.60350(18) 0.14354(17) 0.62348(17) 0.0213(7) Uani 1 1 d . . .
C57 C 0.6529(2) 0.1096(2) 0.68117(19) 0.0314(9) Uani 1 1 d . . .
H57 H 0.6373 0.0929 0.7136 0.038 Uiso 1 1 calc R . .
C58 C 0.7239(2) 0.1002(2) 0.6914(2) 0.0449(12) Uani 1 1 d . . .
H58 H 0.7570 0.0769 0.7308 0.054 Uiso 1 1 calc R . .
C59 C 0.7476(2) 0.1243(2) 0.6451(2) 0.0436(11) Uani 1 1 d . . .
H59 H 0.7969 0.1179 0.6527 0.052 Uiso 1 1 calc R . .
C60 C 0.6992(2) 0.1579(2) 0.5873(2) 0.0380(10) Uani 1 1 d . . .
H60 H 0.7152 0.1741 0.5550 0.046 Uiso 1 1 calc R . .
C61 C 0.62753(19) 0.16768(19) 0.57669(19) 0.0273(8) Uani 1 1 d . . .
H61 H 0.5946 0.1911 0.5372 0.033 Uiso 1 1 calc R . .
C62 C 0.45677(17) 0.14075(18) 0.52423(16) 0.0195(7) Uani 1 1 d . . .
C63 C 0.4331(2) 0.0705(2) 0.50399(18) 0.0283(8) Uani 1 1 d . . .
H63 H 0.4449 0.0332 0.5364 0.034 Uiso 1 1 calc R . .
C64 C 0.3927(2) 0.0545(2) 0.4375(2) 0.0352(9) Uani 1 1 d . . .
H64 H 0.3763 0.0065 0.4246 0.042 Uiso 1 1 calc R . .
C65 C 0.3761(2) 0.1077(2) 0.38977(19) 0.0356(10) Uani 1 1 d . . .
H65 H 0.3479 0.0968 0.3440 0.043 Uiso 1 1 calc R . .
C66 C 0.4010(2) 0.1773(2) 0.40928(19) 0.0339(9) Uani 1 1 d . . .
H66 H 0.3907 0.2140 0.3765 0.041 Uiso 1 1 calc R . .
C67 C 0.44073(19) 0.1939(2) 0.47593(18) 0.0255(8) Uani 1 1 d . . .
H67 H 0.4571 0.2419 0.4887 0.031 Uiso 1 1 calc R . .
C68 C 0.5237(2) 0.46564(18) 0.64543(18) 0.0253(8) Uani 1 1 d . . .
H68A H 0.5234 0.5133 0.6647 0.038 Uiso 1 1 calc R . .
H68B H 0.4930 0.4669 0.5973 0.038 Uiso 1 1 calc R . .
H68C H 0.5735 0.4530 0.6532 0.038 Uiso 1 1 calc R . .
C69 C 0.39944(18) 0.43170(18) 0.67126(16) 0.0205(7) Uani 1 1 d . . .
C70 C 0.34693(19) 0.38395(19) 0.67182(18) 0.0253(8) Uani 1 1 d . . .
H70 H 0.3571 0.3336 0.6771 0.030 Uiso 1 1 calc R . .
C71 C 0.27970(19) 0.4092(2) 0.66466(19) 0.0287(8) Uani 1 1 d . . .
H71 H 0.2443 0.3762 0.6654 0.034 Uiso 1 1 calc R . .
C72 C 0.2639(2) 0.4826(2) 0.65642(19) 0.0293(8) Uani 1 1 d . . .
H72 H 0.2178 0.4998 0.6514 0.035 Uiso 1 1 calc R . .
C73 C 0.3158(2) 0.5301(2) 0.65564(18) 0.0299(9) Uani 1 1 d . . .
H73 H 0.3052 0.5803 0.6496 0.036 Uiso 1 1 calc R . .
C74 C 0.38301(19) 0.50543(18) 0.66359(18) 0.0258(8) Uani 1 1 d . . .
H74 H 0.4186 0.5389 0.6639 0.031 Uiso 1 1 calc R . .
C75 C 0.54085(18) 0.41289(17) 0.77370(17) 0.0201(7) Uani 1 1 d . . .
C76 C 0.5156(2) 0.38511(18) 0.81846(18) 0.0248(8) Uani 1 1 d . . .
H76 H 0.4700 0.3611 0.8020 0.030 Uiso 1 1 calc R . .
C77 C 0.5560(2) 0.3919(2) 0.88651(19) 0.0308(9) Uani 1 1 d . . .
H77 H 0.5381 0.3727 0.9166 0.037 Uiso 1 1 calc R . .
C78 C 0.6226(2) 0.4268(2) 0.91089(19) 0.0320(9) Uani 1 1 d . . .
H78 H 0.6507 0.4310 0.9577 0.038 Uiso 1 1 calc R . .
C79 C 0.64811(19) 0.4553(2) 0.86712(19) 0.0293(9) Uani 1 1 d . . .
H79 H 0.6932 0.4804 0.8838 0.035 Uiso 1 1 calc R . .
C80 C 0.60801(18) 0.44751(18) 0.79872(18) 0.0240(8) Uani 1 1 d . . .
H80 H 0.6265 0.4659 0.7688 0.029 Uiso 1 1 calc R . .
F7 F 0.58720(19) 0.4198(3) 0.46061(18) 0.0625(13) Uani 0.754(4) 1 d PD A 1
F8 F 0.6702(3) 0.3455(3) 0.4807(2) 0.0828(15) Uani 0.754(4) 1 d PDU A 1
F9 F 0.6952(2) 0.4474(3) 0.52973(18) 0.0628(12) Uani 0.754(4) 1 d PDU A 1
F7' F 0.6134(6) 0.4621(7) 0.4936(6) 0.0625(13) Uani 0.246(4) 1 d PD A 2
F8' F 0.6256(10) 0.3571(9) 0.4590(7) 0.0828(15) Uani 0.246(4) 1 d PDU A 2
F9' F 0.7162(7) 0.4026(8) 0.5274(6) 0.0628(12) Uani 0.246(4) 1 d PDU A 2
F10 F 0.33653(12) 0.09137(12) 0.75987(12) 0.0389(6) Uani 1 1 d . A .
F11 F 0.31047(11) 0.19587(12) 0.78424(11) 0.0334(5) Uani 1 1 d . A .
F12 F 0.39109(12) 0.13099(14) 0.86034(11) 0.0436(6) Uani 1 1 d . A .


_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
Os1 C1 1.868(3) . ?
Os1 N4 2.069(3) . ?
Os1 N3 2.081(3) . ?
Os1 N2 2.084(3) . ?
Os1 P2 2.3689(9) . ?
Os1 P1 2.3702(9) . ?
P1 C15 1.813(3) . ?
P1 C16 1.822(3) . ?
P1 C22 1.823(4) . ?
P2 C28 1.815(3) . ?
P2 C29 1.826(3) . ?
P2 C35 1.826(4) . ?
O1 C1 1.151(4) . ?
N1 N2 1.344(4) . ?
N1 C3 1.351(4) . ?
N2 C5 1.365(4) . ?
N3 C6 1.345(4) . ?
N3 C10 1.353(4) . ?
N4 N5 1.341(4) . ?
N4 C11 1.375(4) . ?
N5 C13 1.349(4) . ?
C2 F3 1.338(4) . ?
C2 F2 1.340(4) . ?
C2 F1 1.346(4) . ?
C2 C3 1.474(4) . ?
C3 C4 1.382(5) . ?
C4 C5 1.390(4) . ?
C5 C6 1.452(4) . ?
C6 C7 1.387(4) . ?
C7 C8 1.378(5) . ?
C8 C9 1.387(5) . ?
C9 C10 1.389(5) . ?
C10 C11 1.446(5) . ?
C11 C12 1.382(5) . ?
C12 C13 1.383(5) . ?
C13 C14 1.473(5) . ?
C14 F4' 1.280(13) . ?
C14 F5 1.301(6) . ?
C14 F6 1.336(8) . ?
C14 F6' 1.34(2) . ?
C14 F4 1.383(6) . ?
C14 F5' 1.469(14) . ?
C16 C17 1.384(5) . ?
C16 C21 1.393(5) . ?
C17 C18 1.398(5) . ?
C18 C19 1.380(6) . ?
C19 C20 1.375(6) . ?
C20 C21 1.376(5) . ?
C22 C27 1.384(5) . ?
C22 C23 1.401(5) . ?
C23 C24 1.386(5) . ?
C24 C25 1.379(6) . ?
C25 C26 1.371(6) . ?
C26 C27 1.386(5) . ?
C29 C34 1.380(5) . ?
C29 C30 1.392(5) . ?
C30 C31 1.374(5) . ?
C31 C32 1.380(5) . ?
C32 C33 1.381(5) . ?
C33 C34 1.395(5) . ?
C35 C36 1.383(5) . ?
C35 C40 1.393(5) . ?
C36 C37 1.389(5) . ?
C37 C38 1.378(6) . ?
C38 C39 1.369(6) . ?
C39 C40 1.387(5) . ?
Os2 C41 1.866(3) . ?
Os2 N9 2.070(3) . ?
Os2 N7 2.072(3) . ?
Os2 N8 2.074(3) . ?
Os2 P3 2.3706(8) . ?
Os2 P4 2.3758(8) . ?
P3 C55 1.814(4) . ?
P3 C62 1.826(3) . ?
P3 C56 1.827(3) . ?
P4 C68 1.812(3) . ?
P4 C75 1.822(3) . ?
P4 C69 1.823(3) . ?
O2 C41 1.153(4) . ?
N6 N7 1.342(4) . ?
N6 C43 1.348(4) . ?
N7 C45 1.370(4) . ?
N8 C50 1.352(4) . ?
N8 C46 1.352(4) . ?
N9 N10 1.336(4) . ?
N9 C51 1.370(4) . ?
N10 C53 1.352(4) . ?
C42 F8' 1.286(13) . ?
C42 F9 1.308(5) . ?
C42 F7 1.322(5) . ?
C42 F9' 1.324(12) . ?
C42 F7' 1.359(12) . ?
C42 F8 1.374(6) . ?
C42 C43 1.467(5) . ?
C43 C44 1.378(5) . ?
C44 C45 1.383(5) . ?
C45 C46 1.453(5) . ?
C46 C47 1.386(5) . ?
C47 C48 1.381(5) . ?
C48 C49 1.389(5) . ?
C49 C50 1.392(4) . ?
C50 C51 1.446(5) . ?
C51 C52 1.392(5) . ?
C52 C53 1.384(4) . ?
C53 C54 1.481(5) . ?
C54 F12 1.333(4) . ?
C54 F10 1.339(4) . ?
C54 F11 1.343(4) . ?
C56 C61 1.390(5) . ?
C56 C57 1.395(5) . ?
C57 C58 1.373(6) . ?
C58 C59 1.376(7) . ?
C59 C60 1.387(6) . ?
C60 C61 1.386(5) . ?
C62 C67 1.385(5) . ?
C62 C63 1.393(5) . ?
C63 C64 1.379(5) . ?
C64 C65 1.377(6) . ?
C65 C66 1.384(6) . ?
C66 C67 1.383(5) . ?
C69 C70 1.389(5) . ?
C69 C74 1.398(5) . ?
C70 C71 1.388(5) . ?
C71 C72 1.388(5) . ?
C72 C73 1.379(5) . ?
C73 C74 1.378(5) . ?
C75 C76 1.391(5) . ?
C75 C80 1.393(5) . ?
C76 C77 1.382(5) . ?
C77 C78 1.386(5) . ?
C78 C79 1.381(6) . ?
C79 C80 1.389(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Os1 N4 101.45(13) . . ?
C1 Os1 N3 178.03(13) . . ?
N4 Os1 N3 76.63(10) . . ?
C1 Os1 N2 105.34(13) . . ?
N4 Os1 N2 153.20(10) . . ?
N3 Os1 N2 76.59(10) . . ?
C1 Os1 P2 90.16(11) . . ?
N4 Os1 P2 91.04(8) . . ?
N3 Os1 P2 90.30(8) . . ?
N2 Os1 P2 88.12(8) . . ?
C1 Os1 P1 91.13(11) . . ?
N4 Os1 P1 89.90(8) . . ?
N3 Os1 P1 88.45(8) . . ?
N2 Os1 P1 90.36(8) . . ?
P2 Os1 P1 178.23(3) . . ?
C15 P1 C16 104.72(16) . . ?
C15 P1 C22 104.49(17) . . ?
C16 P1 C22 103.56(16) . . ?
C15 P1 Os1 112.73(13) . . ?
C16 P1 Os1 113.14(11) . . ?
C22 P1 Os1 116.98(12) . . ?
C28 P2 C29 102.63(16) . . ?
C28 P2 C35 105.04(17) . . ?
C29 P2 C35 102.66(16) . . ?
C28 P2 Os1 113.13(12) . . ?
C29 P2 Os1 119.04(11) . . ?
C35 P2 Os1 112.79(11) . . ?
N2 N1 C3 105.2(3) . . ?
N1 N2 C5 110.4(3) . . ?
N1 N2 Os1 134.2(2) . . ?
C5 N2 Os1 115.0(2) . . ?
C6 N3 C10 122.5(3) . . ?
C6 N3 Os1 119.0(2) . . ?
C10 N3 Os1 118.5(2) . . ?
N5 N4 C11 110.4(3) . . ?
N5 N4 Os1 133.4(2) . . ?
C11 N4 Os1 116.1(2) . . ?
N4 N5 C13 105.1(3) . . ?
O1 C1 Os1 178.3(3) . . ?
F3 C2 F2 106.6(3) . . ?
F3 C2 F1 105.6(3) . . ?
F2 C2 F1 106.2(3) . . ?
F3 C2 C3 113.6(3) . . ?
F2 C2 C3 111.5(3) . . ?
F1 C2 C3 112.7(3) . . ?
N1 C3 C4 112.7(3) . . ?
N1 C3 C2 119.0(3) . . ?
C4 C3 C2 128.2(3) . . ?
C3 C4 C5 103.2(3) . . ?
N2 C5 C4 108.5(3) . . ?
N2 C5 C6 117.3(3) . . ?
C4 C5 C6 134.2(3) . . ?
N3 C6 C7 119.7(3) . . ?
N3 C6 C5 111.9(3) . . ?
C7 C6 C5 128.4(3) . . ?
C8 C7 C6 119.0(3) . . ?
C7 C8 C9 120.7(3) . . ?
C8 C9 C10 118.7(3) . . ?
N3 C10 C9 119.4(3) . . ?
N3 C10 C11 112.6(3) . . ?
C9 C10 C11 127.9(3) . . ?
N4 C11 C12 108.2(3) . . ?
N4 C11 C10 116.2(3) . . ?
C12 C11 C10 135.6(3) . . ?
C11 C12 C13 103.5(3) . . ?
N5 C13 C12 112.8(3) . . ?
N5 C13 C14 118.2(3) . . ?
C12 C13 C14 128.8(3) . . ?
F4' C14 F5 79.7(8) . . ?
F4' C14 F6 121.8(11) . . ?
F5 C14 F6 110.3(7) . . ?
F4' C14 F6' 130(3) . . ?
F5 C14 F6' 101(2) . . ?
F6 C14 F6' 12(2) . . ?
F4' C14 F4 30.6(8) . . ?
F5 C14 F4 106.7(4) . . ?
F6 C14 F4 98.2(7) . . ?
F6' C14 F4 109(2) . . ?
F4' C14 F5' 101.5(10) . . ?
F5 C14 F5' 22.2(6) . . ?
F6 C14 F5' 101.6(9) . . ?
F6' C14 F5' 90(2) . . ?
F4 C14 F5' 128.8(7) . . ?
F4' C14 C13 112.0(8) . . ?
F5 C14 C13 115.3(4) . . ?
F6 C14 C13 113.5(9) . . ?
F6' C14 C13 112(3) . . ?
F4 C14 C13 111.4(3) . . ?
F5' C14 C13 103.0(7) . . ?
C17 C16 C21 119.2(3) . . ?
C17 C16 P1 121.6(3) . . ?
C21 C16 P1 119.1(3) . . ?
C16 C17 C18 120.0(4) . . ?
C19 C18 C17 119.6(4) . . ?
C20 C19 C18 120.7(4) . . ?
C19 C20 C21 119.7(4) . . ?
C20 C21 C16 120.8(4) . . ?
C27 C22 C23 118.7(3) . . ?
C27 C22 P1 121.2(3) . . ?
C23 C22 P1 120.1(3) . . ?
C24 C23 C22 120.0(4) . . ?
C25 C24 C23 120.5(4) . . ?
C26 C25 C24 119.6(4) . . ?
C25 C26 C27 120.7(4) . . ?
C22 C27 C26 120.4(4) . . ?
C34 C29 C30 119.4(3) . . ?
C34 C29 P2 121.6(3) . . ?
C30 C29 P2 119.0(3) . . ?
C31 C30 C29 120.4(3) . . ?
C30 C31 C32 120.3(3) . . ?
C31 C32 C33 119.8(3) . . ?
C32 C33 C34 120.1(3) . . ?
C29 C34 C33 120.0(3) . . ?
C36 C35 C40 119.4(3) . . ?
C36 C35 P2 119.3(3) . . ?
C40 C35 P2 121.0(3) . . ?
C35 C36 C37 120.5(3) . . ?
C38 C37 C36 119.4(4) . . ?
C39 C38 C37 120.8(4) . . ?
C38 C39 C40 120.2(4) . . ?
C39 C40 C35 119.7(4) . . ?
C41 Os2 N9 101.79(13) . . ?
C41 Os2 N7 104.74(13) . . ?
N9 Os2 N7 153.47(10) . . ?
C41 Os2 N8 177.77(13) . . ?
N9 Os2 N8 76.63(11) . . ?
N7 Os2 N8 76.87(11) . . ?
C41 Os2 P3 92.20(10) . . ?
N9 Os2 P3 89.81(8) . . ?
N7 Os2 P3 88.81(8) . . ?
N8 Os2 P3 89.37(7) . . ?
C41 Os2 P4 89.55(10) . . ?
N9 Os2 P4 92.60(8) . . ?
N7 Os2 P4 88.00(8) . . ?
N8 Os2 P4 88.96(7) . . ?
P3 Os2 P4 176.67(3) . . ?
C55 P3 C62 105.07(16) . . ?
C55 P3 C56 104.26(17) . . ?
C62 P3 C56 103.04(15) . . ?
C55 P3 Os2 113.30(13) . . ?
C62 P3 Os2 116.98(11) . . ?
C56 P3 Os2 112.88(11) . . ?
C68 P4 C75 104.69(16) . . ?
C68 P4 C69 104.91(16) . . ?
C75 P4 C69 101.83(15) . . ?
C68 P4 Os2 112.59(12) . . ?
C75 P4 Os2 114.02(10) . . ?
C69 P4 Os2 117.41(11) . . ?
N7 N6 C43 105.2(3) . . ?
N6 N7 C45 110.1(3) . . ?
N6 N7 Os2 134.5(2) . . ?
C45 N7 Os2 115.4(2) . . ?
C50 N8 C46 122.3(3) . . ?
C50 N8 Os2 118.8(2) . . ?
C46 N8 Os2 118.9(2) . . ?
N10 N9 C51 110.6(3) . . ?
N10 N9 Os2 133.5(2) . . ?
C51 N9 Os2 115.8(2) . . ?
N9 N10 C53 105.4(3) . . ?
O2 C41 Os2 177.7(3) . . ?
F8' C42 F9 126.6(8) . . ?
F8' C42 F7 65.2(8) . . ?
F9 C42 F7 108.8(4) . . ?
F8' C42 F9' 100.6(10) . . ?
F9 C42 F9' 42.1(6) . . ?
F7 C42 F9' 132.8(7) . . ?
F8' C42 F7' 108.0(10) . . ?
F9 C42 F7' 70.1(6) . . ?
F7 C42 F7' 46.0(5) . . ?
F9' C42 F7' 109.7(8) . . ?
F8' C42 F8 37.3(8) . . ?
F9 C42 F8 104.9(4) . . ?
F7 C42 F8 100.4(4) . . ?
F9' C42 F8 67.3(7) . . ?
F7' C42 F8 134.2(6) . . ?
F8' C42 C43 114.3(8) . . ?
F9 C42 C43 115.3(3) . . ?
F7 C42 C43 114.8(3) . . ?
F9' C42 C43 112.0(6) . . ?
F7' C42 C43 111.7(6) . . ?
F8 C42 C43 111.1(4) . . ?
N6 C43 C44 112.9(3) . . ?
N6 C43 C42 119.6(3) . . ?
C44 C43 C42 127.5(3) . . ?
C43 C44 C45 103.3(3) . . ?
N7 C45 C44 108.6(3) . . ?
N7 C45 C46 116.9(3) . . ?
C44 C45 C46 134.5(3) . . ?
N8 C46 C47 119.9(3) . . ?
N8 C46 C45 111.9(3) . . ?
C47 C46 C45 128.3(3) . . ?
C48 C47 C46 118.8(3) . . ?
C47 C48 C49 120.9(3) . . ?
C48 C49 C50 118.5(3) . . ?
N8 C50 C49 119.6(3) . . ?
N8 C50 C51 112.2(3) . . ?
C49 C50 C51 128.1(3) . . ?
N9 C51 C52 108.2(3) . . ?
N9 C51 C50 116.5(3) . . ?
C52 C51 C50 135.3(3) . . ?
C53 C52 C51 103.3(3) . . ?
N10 C53 C52 112.5(3) . . ?
N10 C53 C54 119.1(3) . . ?
C52 C53 C54 128.5(3) . . ?
F12 C54 F10 107.1(3) . . ?
F12 C54 F11 107.0(3) . . ?
F10 C54 F11 105.4(3) . . ?
F12 C54 C53 111.6(3) . . ?
F10 C54 C53 112.6(3) . . ?
F11 C54 C53 112.8(3) . . ?
C61 C56 C57 118.8(3) . . ?
C61 C56 P3 120.3(3) . . ?
C57 C56 P3 120.8(3) . . ?
C58 C57 C56 120.5(4) . . ?
C57 C58 C59 120.7(4) . . ?
C58 C59 C60 119.7(4) . . ?
C61 C60 C59 120.0(4) . . ?
C60 C61 C56 120.4(4) . . ?
C67 C62 C63 118.5(3) . . ?
C67 C62 P3 120.5(3) . . ?
C63 C62 P3 120.9(3) . . ?
C64 C63 C62 120.8(4) . . ?
C65 C64 C63 120.4(4) . . ?
C64 C65 C66 119.1(4) . . ?
C67 C66 C65 120.7(4) . . ?
C66 C67 C62 120.3(3) . . ?
C70 C69 C74 118.5(3) . . ?
C70 C69 P4 120.3(3) . . ?
C74 C69 P4 121.2(3) . . ?
C71 C70 C69 120.5(3) . . ?
C70 C71 C72 120.4(3) . . ?
C73 C72 C71 119.4(3) . . ?
C74 C73 C72 120.5(3) . . ?
C73 C74 C69 120.8(3) . . ?
C76 C75 C80 118.7(3) . . ?
C76 C75 P4 120.0(3) . . ?
C80 C75 P4 121.2(3) . . ?
C77 C76 C75 120.9(3) . . ?
C76 C77 C78 120.0(4) . . ?
C79 C78 C77 119.9(3) . . ?
C78 C79 C80 120.1(3) . . ?
C79 C80 C75 120.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.655
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 989383'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H40 F6 N6 O2 Os P2'
_chemical_formula_weight         1099.00

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'
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'
Os Os -1.2165 7.6030 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   12.6562(6)
_cell_length_b                   14.1830(7)
_cell_length_c                   14.3426(7)
_cell_angle_alpha                67.8740(10)
_cell_angle_beta                 82.5019(11)
_cell_angle_gamma                67.8270(10)
_cell_volume                     2208.37(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7147
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      24.67

_exptl_crystal_description       block
_exptl_crystal_colour            deep-yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    3.033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5177
_exptl_absorpt_correction_T_max  0.5822
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24937
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         27.50
_reflns_number_total             10127
_reflns_number_gt                9186
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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     
'calc w=1/[σ²(Fo²)+(0.0437P)²+0.0000P] 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         10127
_refine_ls_number_parameters     588
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0835
_refine_ls_wR_factor_gt          0.0812
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.181935(10) 0.278369(10) 0.315174(10) 0.01685(5) Uani 1 1 d . . .
P1 P 0.07146(8) 0.18233(7) 0.41511(7) 0.01916(18) Uani 1 1 d . . .
P2 P 0.33176(8) 0.32646(8) 0.23002(7) 0.02011(19) Uani 1 1 d . . .
N1 N 0.2860(2) 0.3056(3) 0.4875(2) 0.0238(7) Uani 1 1 d . . .
N2 N 0.2066(2) 0.3394(2) 0.4170(2) 0.0199(6) Uani 1 1 d . . .
N3 N 0.0613(2) 0.4290(2) 0.2713(2) 0.0195(6) Uani 1 1 d . . .
N4 N 0.1054(2) 0.2807(2) 0.1954(2) 0.0208(6) Uani 1 1 d . . .
N5 N 0.1112(3) 0.2040(3) 0.1590(2) 0.0251(7) Uani 1 1 d . . .
N6 N 0.3090(2) 0.1222(2) 0.3603(2) 0.0202(6) Uani 1 1 d . . .
C1 C 0.3398(4) 0.3767(4) 0.5953(4) 0.0447(12) Uani 1 1 d . . .
C2 C 0.2631(3) 0.3903(3) 0.5183(3) 0.0277(8) Uani 1 1 d . . .
C3 C 0.1699(3) 0.4787(3) 0.4695(3) 0.0276(8) Uani 1 1 d . . .
H3 H 0.1369 0.5467 0.4790 0.033 Uiso 1 1 calc R . .
C4 C 0.1350(3) 0.4448(3) 0.4028(3) 0.0216(7) Uani 1 1 d . . .
C5 C 0.0508(3) 0.4952(3) 0.3230(3) 0.0232(8) Uani 1 1 d . . .
C6 C -0.0320(3) 0.5992(3) 0.2931(3) 0.0289(9) Uani 1 1 d . . .
H6 H -0.0402 0.6463 0.3283 0.035 Uiso 1 1 calc R . .
C7 C -0.1020(3) 0.6333(3) 0.2118(3) 0.0327(9) Uani 1 1 d . . .
H7 H -0.1589 0.7042 0.1912 0.039 Uiso 1 1 calc R . .
C8 C -0.0900(3) 0.5648(3) 0.1599(3) 0.0293(9) Uani 1 1 d . . .
H8 H -0.1380 0.5885 0.1036 0.035 Uiso 1 1 calc R . .
C9 C -0.0072(3) 0.4615(3) 0.1914(3) 0.0227(7) Uani 1 1 d . . .
C10 C 0.0164(3) 0.3751(3) 0.1512(3) 0.0232(8) Uani 1 1 d . . .
C11 C -0.0363(3) 0.3599(3) 0.0822(3) 0.0290(9) Uani 1 1 d . . .
H11 H -0.0997 0.4109 0.0393 0.035 Uiso 1 1 calc R . .
C12 C 0.0248(3) 0.2534(3) 0.0903(3) 0.0283(8) Uani 1 1 d . . .
C13 C 0.0069(4) 0.1895(4) 0.0375(4) 0.0406(11) Uani 1 1 d . . .
C14 C 0.1574(3) 0.0477(3) 0.4086(3) 0.0240(8) Uani 1 1 d . . .
H14A H 0.1424 -0.0098 0.4682 0.029 Uiso 1 1 calc R . .
H14B H 0.1355 0.0421 0.3477 0.029 Uiso 1 1 calc R . .
C15 C 0.2821(3) 0.0309(3) 0.4053(3) 0.0232(8) Uani 1 1 d . . .
C16 C 0.3643(3) -0.0718(3) 0.4393(3) 0.0298(9) Uani 1 1 d . . .
H16 H 0.3426 -0.1335 0.4733 0.036 Uiso 1 1 calc R . .
C17 C 0.4787(4) -0.0853(3) 0.4238(3) 0.0338(9) Uani 1 1 d . . .
H17 H 0.5364 -0.1557 0.4458 0.041 Uiso 1 1 calc R . .
C18 C 0.5064(3) 0.0064(3) 0.3758(3) 0.0290(9) Uani 1 1 d . . .
H18 H 0.5841 -0.0005 0.3630 0.035 Uiso 1 1 calc R . .
C19 C 0.4218(3) 0.1086(3) 0.3460(3) 0.0231(8) Uani 1 1 d . . .
C20 C 0.4512(3) 0.2091(3) 0.3053(3) 0.0265(8) Uani 1 1 d . . .
H20A H 0.5197 0.1971 0.2628 0.032 Uiso 1 1 calc R . .
H20B H 0.4694 0.2248 0.3617 0.032 Uiso 1 1 calc R . .
C21 C -0.0689(3) 0.2127(3) 0.3679(3) 0.0215(7) Uani 1 1 d . . .
C22 C -0.0952(3) 0.1407(3) 0.3389(3) 0.0278(8) Uani 1 1 d . . .
H22 H -0.0418 0.0688 0.3511 0.033 Uiso 1 1 calc R . .
C23 C -0.1987(3) 0.1732(4) 0.2924(3) 0.0349(10) Uani 1 1 d . . .
H23 H -0.2159 0.1233 0.2732 0.042 Uiso 1 1 calc R . .
C24 C -0.2773(3) 0.2774(4) 0.2737(4) 0.0349(10) Uani 1 1 d . . .
H24 H -0.3476 0.2998 0.2405 0.042 Uiso 1 1 calc R . .
C25 C -0.2528(3) 0.3489(3) 0.3035(3) 0.0333(9) Uani 1 1 d . . .
H25 H -0.3067 0.4205 0.2916 0.040 Uiso 1 1 calc R . .
C26 C -0.1497(3) 0.3163(3) 0.3510(3) 0.0291(9) Uani 1 1 d . . .
H26 H -0.1341 0.3656 0.3722 0.035 Uiso 1 1 calc R . .
C27 C 0.0546(3) 0.1615(3) 0.5485(3) 0.0227(8) Uani 1 1 d . . .
C28 C -0.0475(4) 0.1665(3) 0.5994(3) 0.0303(9) Uani 1 1 d . . .
H28 H -0.1147 0.1839 0.5640 0.036 Uiso 1 1 calc R . .
C29 C -0.0512(4) 0.1461(4) 0.7023(3) 0.0395(11) Uani 1 1 d . . .
H29 H -0.1207 0.1481 0.7373 0.047 Uiso 1 1 calc R . .
C30 C 0.0452(4) 0.1229(3) 0.7537(3) 0.0409(11) Uani 1 1 d . . .
H30 H 0.0420 0.1094 0.8239 0.049 Uiso 1 1 calc R . .
C31 C 0.1464(4) 0.1192(3) 0.7039(3) 0.0365(10) Uani 1 1 d . . .
H31 H 0.2129 0.1030 0.7396 0.044 Uiso 1 1 calc R . .
C32 C 0.1511(3) 0.1392(3) 0.6018(3) 0.0283(8) Uani 1 1 d . . .
H32 H 0.2208 0.1376 0.5675 0.034 Uiso 1 1 calc R . .
C33 C 0.3632(3) 0.3350(3) 0.1000(3) 0.0221(7) Uani 1 1 d . . .
C34 C 0.3456(3) 0.2591(3) 0.0708(3) 0.0272(8) Uani 1 1 d . . .
H34 H 0.3167 0.2068 0.1178 0.033 Uiso 1 1 calc R . .
C35 C 0.3696(3) 0.2587(4) -0.0256(3) 0.0328(9) Uani 1 1 d . . .
H35 H 0.3573 0.2063 -0.0446 0.039 Uiso 1 1 calc R . .
C36 C 0.4113(3) 0.3340(4) -0.0943(3) 0.0340(9) Uani 1 1 d . . .
H36 H 0.4287 0.3327 -0.1604 0.041 Uiso 1 1 calc R . .
C37 C 0.4281(4) 0.4113(4) -0.0681(3) 0.0386(10) Uani 1 1 d . . .
H37 H 0.4556 0.4640 -0.1162 0.046 Uiso 1 1 calc R . .
C38 C 0.4043(4) 0.4119(3) 0.0296(3) 0.0320(9) Uani 1 1 d . . .
H38 H 0.4163 0.4648 0.0481 0.038 Uiso 1 1 calc R . .
C39 C 0.3472(3) 0.4456(3) 0.2383(3) 0.0234(8) Uani 1 1 d . . .
C40 C 0.4234(3) 0.4404(3) 0.3029(3) 0.0266(8) Uani 1 1 d . . .
H40 H 0.4771 0.3718 0.3407 0.032 Uiso 1 1 calc R . .
C41 C 0.4219(3) 0.5348(4) 0.3129(3) 0.0325(9) Uani 1 1 d . . .
H41 H 0.4744 0.5303 0.3575 0.039 Uiso 1 1 calc R . .
C42 C 0.3448(4) 0.6345(4) 0.2585(4) 0.0381(10) Uani 1 1 d . . .
H42 H 0.3440 0.6987 0.2658 0.046 Uiso 1 1 calc R . .
C43 C 0.2684(4) 0.6418(3) 0.1933(3) 0.0367(10) Uani 1 1 d . . .
H43 H 0.2156 0.7108 0.1552 0.044 Uiso 1 1 calc R . .
C44 C 0.2689(3) 0.5477(3) 0.1836(3) 0.0305(9) Uani 1 1 d . . .
H44 H 0.2156 0.5528 0.1395 0.037 Uiso 1 1 calc R . .
F1 F 0.4484(2) 0.3571(3) 0.5651(2) 0.0536(8) Uani 1 1 d . . .
F2 F 0.3471(3) 0.2906(3) 0.6815(2) 0.0685(9) Uani 1 1 d . . .
F3 F 0.3070(3) 0.4622(3) 0.6222(3) 0.0975(16) Uani 1 1 d . . .
F4 F -0.0112(3) 0.1007(3) 0.0990(2) 0.0680(10) Uani 1 1 d . . .
F5 F 0.0954(3) 0.1547(3) -0.0194(2) 0.0667(9) Uani 1 1 d . . .
F6 F -0.0811(3) 0.2470(3) -0.0258(3) 0.0845(13) Uani 1 1 d . . .
O1 O 0.6548(5) -0.0202(5) 0.0914(5) 0.116(2) Uani 1 1 d . . .
O2 O 0.6752(4) 0.0932(3) -0.0623(3) 0.0803(14) Uani 1 1 d D . .
C45 C 0.6686(5) 0.0640(6) 0.0374(5) 0.0726(18) Uani 1 1 d . . .
C46 C 0.6805(5) 0.1459(6) 0.0705(5) 0.0711(18) Uani 1 1 d . . .
H46A H 0.6540 0.1344 0.1399 0.107 Uiso 1 1 calc R . .
H46B H 0.6346 0.2190 0.0264 0.107 Uiso 1 1 calc R . .
H46C H 0.7608 0.1389 0.0673 0.107 Uiso 1 1 calc R . .
C47 C 0.6513(8) 0.0209(6) -0.0900(6) 0.121(4) Uani 1 1 d D . .
H47A H 0.5891 0.0013 -0.0476 0.145 Uiso 1 1 calc R . .
H47B H 0.7196 -0.0465 -0.0773 0.145 Uiso 1 1 calc R . .
C48 C 0.6186(8) 0.0627(6) -0.1921(6) 0.122(4) Uani 1 1 d D . .
H48A H 0.6071 0.0064 -0.2090 0.183 Uiso 1 1 calc R . .
H48B H 0.6786 0.0849 -0.2344 0.183 Uiso 1 1 calc R . .
H48C H 0.5474 0.1259 -0.2039 0.183 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os N3 2.017(3) . ?
Os N2 2.063(3) . ?
Os N4 2.063(3) . ?
Os N6 2.102(3) . ?
Os P2 2.3015(9) . ?
Os P1 2.3041(9) . ?
P1 C27 1.819(4) . ?
P1 C21 1.821(4) . ?
P1 C14 1.838(4) . ?
P2 C39 1.821(4) . ?
P2 C33 1.823(4) . ?
P2 C20 1.842(4) . ?
N1 N2 1.341(4) . ?
N1 C2 1.351(5) . ?
N2 C4 1.376(4) . ?
N3 C9 1.355(5) . ?
N3 C5 1.362(5) . ?
N4 N5 1.350(4) . ?
N4 C10 1.368(5) . ?
N5 C12 1.356(5) . ?
N6 C15 1.362(5) . ?
N6 C19 1.364(4) . ?
C1 F3 1.312(5) . ?
C1 F1 1.343(5) . ?
C1 F2 1.356(6) . ?
C1 C2 1.475(6) . ?
C2 C3 1.375(5) . ?
C3 C4 1.399(5) . ?
C4 C5 1.444(5) . ?
C5 C6 1.389(5) . ?
C6 C7 1.378(6) . ?
C7 C8 1.387(6) . ?
C8 C9 1.384(5) . ?
C9 C10 1.460(5) . ?
C10 C11 1.383(5) . ?
C11 C12 1.379(6) . ?
C12 C13 1.471(6) . ?
C13 F4 1.322(5) . ?
C13 F6 1.324(5) . ?
C13 F5 1.347(6) . ?
C14 C15 1.501(5) . ?
C15 C16 1.377(5) . ?
C16 C17 1.387(6) . ?
C17 C18 1.377(6) . ?
C18 C19 1.383(5) . ?
C19 C20 1.492(5) . ?
C21 C26 1.387(5) . ?
C21 C22 1.393(5) . ?
C22 C23 1.383(5) . ?
C23 C24 1.381(6) . ?
C24 C25 1.380(6) . ?
C25 C26 1.385(5) . ?
C27 C28 1.390(5) . ?
C27 C32 1.394(5) . ?
C28 C29 1.391(6) . ?
C29 C30 1.375(7) . ?
C30 C31 1.375(6) . ?
C31 C32 1.380(6) . ?
C33 C34 1.389(5) . ?
C33 C38 1.393(5) . ?
C34 C35 1.377(5) . ?
C35 C36 1.373(6) . ?
C36 C37 1.377(6) . ?
C37 C38 1.396(6) . ?
C39 C40 1.386(5) . ?
C39 C44 1.399(5) . ?
C40 C41 1.393(5) . ?
C41 C42 1.373(6) . ?
C42 C43 1.381(6) . ?
C43 C44 1.390(5) . ?
O1 C45 1.217(8) . ?
O2 C45 1.331(8) . ?
O2 C47 1.368(6) . ?
C45 C46 1.471(9) . ?
C47 C48 1.410(7) . ?

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
N3 Os N2 78.08(12) . . ?
N3 Os N4 78.02(12) . . ?
N2 Os N4 156.09(12) . . ?
N3 Os N6 179.36(11) . . ?
N2 Os N6 101.71(11) . . ?
N4 Os N6 102.19(11) . . ?
N3 Os P2 97.30(8) . . ?
N2 Os P2 85.30(8) . . ?
N4 Os P2 98.11(8) . . ?
N6 Os P2 82.08(9) . . ?
N3 Os P1 98.85(8) . . ?
N2 Os P1 97.63(8) . . ?
N4 Os P1 85.66(8) . . ?
N6 Os P1 81.77(9) . . ?
P2 Os P1 163.85(3) . . ?
C27 P1 C21 106.11(17) . . ?
C27 P1 C14 105.72(17) . . ?
C21 P1 C14 104.51(17) . . ?
C27 P1 Os 121.30(12) . . ?
C21 P1 Os 118.22(12) . . ?
C14 P1 Os 98.58(12) . . ?
C39 P2 C33 105.70(17) . . ?
C39 P2 C20 105.30(17) . . ?
C33 P2 C20 105.35(17) . . ?
C39 P2 Os 116.81(12) . . ?
C33 P2 Os 122.33(12) . . ?
C20 P2 Os 99.22(12) . . ?
N2 N1 C2 105.5(3) . . ?
N1 N2 C4 110.4(3) . . ?
N1 N2 Os 134.7(2) . . ?
C4 N2 Os 114.3(2) . . ?
C9 N3 C5 121.8(3) . . ?
C9 N3 Os 119.2(2) . . ?
C5 N3 Os 119.0(2) . . ?
N5 N4 C10 110.4(3) . . ?
N5 N4 Os 134.1(2) . . ?
C10 N4 Os 114.7(2) . . ?
N4 N5 C12 104.9(3) . . ?
C15 N6 C19 117.6(3) . . ?
C15 N6 Os 121.3(2) . . ?
C19 N6 Os 121.1(2) . . ?
F3 C1 F1 108.1(4) . . ?
F3 C1 F2 105.8(4) . . ?
F1 C1 F2 103.5(4) . . ?
F3 C1 C2 112.2(4) . . ?
F1 C1 C2 112.8(4) . . ?
F2 C1 C2 113.9(4) . . ?
N1 C2 C3 112.7(3) . . ?
N1 C2 C1 117.4(4) . . ?
C3 C2 C1 129.9(4) . . ?
C2 C3 C4 103.7(3) . . ?
N2 C4 C3 107.7(3) . . ?
N2 C4 C5 116.5(3) . . ?
C3 C4 C5 135.7(3) . . ?
N3 C5 C6 119.3(4) . . ?
N3 C5 C4 112.0(3) . . ?
C6 C5 C4 128.6(3) . . ?
C7 C6 C5 119.5(4) . . ?
C6 C7 C8 120.5(4) . . ?
C9 C8 C7 119.0(4) . . ?
N3 C9 C8 119.9(3) . . ?
N3 C9 C10 111.9(3) . . ?
C8 C9 C10 128.1(4) . . ?
N4 C10 C11 108.4(3) . . ?
N4 C10 C9 116.1(3) . . ?
C11 C10 C9 135.3(4) . . ?
C12 C11 C10 103.8(3) . . ?
N5 C12 C11 112.5(3) . . ?
N5 C12 C13 118.3(4) . . ?
C11 C12 C13 129.2(4) . . ?
F4 C13 F6 107.1(4) . . ?
F4 C13 F5 105.3(4) . . ?
F6 C13 F5 104.7(4) . . ?
F4 C13 C12 113.3(4) . . ?
F6 C13 C12 111.9(4) . . ?
F5 C13 C12 113.9(4) . . ?
C15 C14 P1 110.3(2) . . ?
N6 C15 C16 122.2(3) . . ?
N6 C15 C14 116.1(3) . . ?
C16 C15 C14 121.5(3) . . ?
C15 C16 C17 120.0(4) . . ?
C18 C17 C16 118.1(4) . . ?
C17 C18 C19 120.3(4) . . ?
N6 C19 C18 121.8(3) . . ?
N6 C19 C20 117.2(3) . . ?
C18 C19 C20 120.8(3) . . ?
C19 C20 P2 110.8(2) . . ?
C26 C21 C22 118.4(3) . . ?
C26 C21 P1 118.3(3) . . ?
C22 C21 P1 123.0(3) . . ?
C23 C22 C21 120.3(4) . . ?
C24 C23 C22 120.7(4) . . ?
C25 C24 C23 119.4(4) . . ?
C24 C25 C26 120.0(4) . . ?
C25 C26 C21 121.1(4) . . ?
C28 C27 C32 118.8(4) . . ?
C28 C27 P1 124.1(3) . . ?
C32 C27 P1 117.1(3) . . ?
C27 C28 C29 119.9(4) . . ?
C30 C29 C28 120.3(4) . . ?
C29 C30 C31 120.3(4) . . ?
C30 C31 C32 119.9(4) . . ?
C31 C32 C27 120.8(4) . . ?
C34 C33 C38 118.8(3) . . ?
C34 C33 P2 117.3(3) . . ?
C38 C33 P2 123.9(3) . . ?
C35 C34 C33 120.8(4) . . ?
C36 C35 C34 120.1(4) . . ?
C35 C36 C37 120.5(4) . . ?
C36 C37 C38 119.7(4) . . ?
C33 C38 C37 120.1(4) . . ?
C40 C39 C44 118.5(3) . . ?
C40 C39 P2 123.9(3) . . ?
C44 C39 P2 117.2(3) . . ?
C39 C40 C41 120.6(4) . . ?
C42 C41 C40 120.2(4) . . ?
C41 C42 C43 120.2(4) . . ?
C42 C43 C44 119.8(4) . . ?
C43 C44 C39 120.7(4) . . ?
C45 O2 C47 108.6(6) . . ?
O1 C45 O2 122.8(7) . . ?
O1 C45 C46 126.3(7) . . ?
O2 C45 C46 111.0(6) . . ?
O2 C47 C48 112.8(6) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.127
_database_code_depnum_ccdc_archive 'CCDC 989384'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H50 F12 N16 O7 Os2'
_chemical_formula_weight         1763.60

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'
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

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

_cell_length_a                   10.9693(5)
_cell_length_b                   16.5070(7)
_cell_length_c                   20.1948(9)
_cell_angle_alpha                71.3583(10)
_cell_angle_beta                 75.9862(10)
_cell_angle_gamma                72.9983(10)
_cell_volume                     3268.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7798
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      24.63

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1724
_exptl_absorpt_coefficient_mu    3.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2986
_exptl_absorpt_correction_T_max  0.6683
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42575
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.08
_diffrn_reflns_theta_max         27.50
_reflns_number_total             14979
_reflns_number_gt                12419
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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. The isotropic restraints 
 are used to the disordered F atoms. 
;

_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)+(0.0247P)²+7.0789P] 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         14979
_refine_ls_number_parameters     933
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0831
_refine_ls_wR_factor_gt          0.0753
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.016
_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
Os1 Os 0.014713(17) 0.729368(12) 0.491739(9) 0.01602(5) Uani 1 1 d . . .
N1 N -0.1696(4) 0.8109(3) 0.5192(2) 0.0207(9) Uani 1 1 d . . .
N2 N 0.0596(4) 0.8065(2) 0.5435(2) 0.0171(8) Uani 1 1 d . . .
N3 N 0.3877(4) 0.7350(3) 0.5072(3) 0.0299(10) Uani 1 1 d . . .
N4 N -0.0292(4) 0.5951(3) 0.6428(2) 0.0207(9) Uani 1 1 d . . .
N5 N -0.0411(4) 0.6277(3) 0.5740(2) 0.0191(8) Uani 1 1 d . . .
N6 N -0.0667(4) 0.6746(3) 0.4425(2) 0.0182(8) Uani 1 1 d . . .
N7 N 0.0272(4) 0.8127(3) 0.3901(2) 0.0201(9) Uani 1 1 d . . .
N8 N 0.0826(4) 0.8803(3) 0.3553(2) 0.0227(9) Uani 1 1 d . . .
C1 C 0.1774(5) 0.6635(3) 0.4651(3) 0.0199(10) Uani 1 1 d . . .
C2 C -0.2825(5) 0.8048(3) 0.5094(3) 0.0268(11) Uani 1 1 d . . .
H2 H -0.2827 0.7609 0.4884 0.032 Uiso 1 1 calc R . .
C3 C -0.3983(5) 0.8594(4) 0.5286(3) 0.0321(13) Uani 1 1 d . . .
H3 H -0.4773 0.8528 0.5219 0.039 Uiso 1 1 calc R . .
C4 C -0.3973(5) 0.9238(4) 0.5577(3) 0.0328(13) Uani 1 1 d . . .
H4 H -0.4760 0.9625 0.5712 0.039 Uiso 1 1 calc R . .
C5 C -0.2823(5) 0.9321(3) 0.5674(3) 0.0276(12) Uani 1 1 d . . .
H5 H -0.2806 0.9766 0.5873 0.033 Uiso 1 1 calc R . .
C6 C -0.1683(5) 0.8745(3) 0.5474(3) 0.0217(10) Uani 1 1 d . . .
C7 C -0.0397(5) 0.8753(3) 0.5577(2) 0.0200(10) Uani 1 1 d . . .
C8 C -0.0218(5) 0.9402(3) 0.5814(3) 0.0243(11) Uani 1 1 d . . .
H8 H -0.0931 0.9864 0.5910 0.029 Uiso 1 1 calc R . .
C9 C 0.0989(5) 0.9380(3) 0.5910(3) 0.0246(11) Uani 1 1 d . . .
H9 H 0.1134 0.9836 0.6051 0.030 Uiso 1 1 calc R . .
C10 C 0.1984(5) 0.8676(3) 0.5797(3) 0.0232(11) Uani 1 1 d . . .
H10 H 0.2825 0.8640 0.5869 0.028 Uiso 1 1 calc R . .
C11 C 0.1767(5) 0.8018(3) 0.5580(2) 0.0195(10) Uani 1 1 d . . .
C12 C 0.2819(5) 0.7223(3) 0.5544(3) 0.0222(11) Uani 1 1 d . . .
C13 C 0.2718(5) 0.6412(3) 0.6016(3) 0.0271(12) Uani 1 1 d . . .
H13 H 0.1946 0.6346 0.6343 0.032 Uiso 1 1 calc R . .
C14 C 0.3759(5) 0.5711(4) 0.6000(3) 0.0335(13) Uani 1 1 d . . .
H14 H 0.3727 0.5153 0.6325 0.040 Uiso 1 1 calc R . .
C15 C 0.4853(5) 0.5824(4) 0.5505(3) 0.0367(14) Uani 1 1 d . . .
H15 H 0.5580 0.5345 0.5480 0.044 Uiso 1 1 calc R . .
C16 C 0.4871(5) 0.6646(4) 0.5048(3) 0.0332(13) Uani 1 1 d . . .
H16 H 0.5618 0.6718 0.4702 0.040 Uiso 1 1 calc R . .
C17 C -0.0910(5) 0.4759(3) 0.7423(3) 0.0268(11) Uani 1 1 d . . .
C18 C -0.0886(5) 0.5273(3) 0.6673(3) 0.0234(11) Uani 1 1 d . . .
C19 C -0.1371(5) 0.5147(3) 0.6153(3) 0.0225(11) Uani 1 1 d . . .
H19 H -0.1822 0.4717 0.6194 0.027 Uiso 1 1 calc R . .
C20 C -0.1042(4) 0.5798(3) 0.5556(3) 0.0192(10) Uani 1 1 d . . .
C21 C -0.1206(4) 0.6058(3) 0.4816(3) 0.0197(10) Uani 1 1 d . . .
C22 C -0.1833(5) 0.5710(3) 0.4488(3) 0.0253(11) Uani 1 1 d . . .
H22 H -0.2189 0.5217 0.4748 0.030 Uiso 1 1 calc R . .
C23 C -0.1930(5) 0.6089(4) 0.3782(3) 0.0287(12) Uani 1 1 d . . .
H23 H -0.2343 0.5849 0.3552 0.034 Uiso 1 1 calc R . .
C24 C -0.1432(5) 0.6820(3) 0.3404(3) 0.0260(11) Uani 1 1 d . . .
H24 H -0.1528 0.7093 0.2922 0.031 Uiso 1 1 calc R . .
C25 C -0.0798(5) 0.7141(3) 0.3736(3) 0.0228(11) Uani 1 1 d . . .
C26 C -0.0210(5) 0.7899(3) 0.3439(3) 0.0217(10) Uani 1 1 d . . .
C27 C 0.0026(5) 0.8455(3) 0.2771(3) 0.0253(11) Uani 1 1 d . . .
H27 H -0.0199 0.8459 0.2344 0.030 Uiso 1 1 calc R . .
C28 C 0.0671(5) 0.9005(3) 0.2870(3) 0.0267(11) Uani 1 1 d . . .
C29 C 0.1241(7) 0.9704(4) 0.2334(3) 0.0388(15) Uani 1 1 d . . .
O1 O 0.2751(3) 0.6229(2) 0.44369(19) 0.0282(8) Uani 1 1 d . . .
F1 F 0.0247(3) 0.4475(2) 0.76229(16) 0.0399(8) Uani 1 1 d . . .
F2 F -0.1364(4) 0.4045(2) 0.75519(18) 0.0474(9) Uani 1 1 d . . .
F3 F -0.1663(3) 0.5208(2) 0.78818(16) 0.0413(8) Uani 1 1 d . . .
F4 F 0.2473(4) 0.9414(3) 0.2074(2) 0.0795(15) Uani 1 1 d . . .
F5 F 0.0634(5) 1.0047(3) 0.1778(2) 0.0746(14) Uani 1 1 d . . .
F6 F 0.1226(4) 1.0353(2) 0.25852(19) 0.0567(11) Uani 1 1 d . . .
Os2 Os 0.302743(17) 1.269010(12) 0.077363(9) 0.01596(5) Uani 1 1 d . . .
N9 N 0.1906(4) 1.4013(3) 0.0575(2) 0.0206(9) Uani 1 1 d . . .
N10 N 0.4262(4) 1.3366(3) -0.0045(2) 0.0184(8) Uani 1 1 d . . .
N11 N 0.6949(4) 1.1658(3) 0.0010(3) 0.0336(11) Uani 1 1 d . . .
N12 N 0.4479(4) 1.3130(3) 0.1755(2) 0.0239(9) Uani 1 1 d . . .
N13 N 0.3480(4) 1.2910(2) 0.1630(2) 0.0185(8) Uani 1 1 d . . .
N14 N 0.1566(4) 1.2352(2) 0.1550(2) 0.0165(8) Uani 1 1 d . A .
N15 N 0.1919(4) 1.2381(3) 0.0226(2) 0.0198(9) Uani 1 1 d . . .
N16 N 0.2031(4) 1.2301(3) -0.0428(2) 0.0220(9) Uani 1 1 d . . .
C30 C 0.4063(5) 1.1561(3) 0.0968(3) 0.0199(10) Uani 1 1 d . . .
C31 C 0.0698(5) 1.4294(3) 0.0899(3) 0.0246(11) Uani 1 1 d . . .
H31 H 0.0241 1.3869 0.1204 0.030 Uiso 1 1 calc R . .
C32 C 0.0096(5) 1.5174(4) 0.0806(3) 0.0290(12) Uani 1 1 d . . .
H32 H -0.0757 1.5350 0.1043 0.035 Uiso 1 1 calc R . .
C33 C 0.0749(6) 1.5785(3) 0.0368(3) 0.0317(13) Uani 1 1 d . . .
H33 H 0.0361 1.6395 0.0302 0.038 Uiso 1 1 calc R . .
C34 C 0.1978(6) 1.5511(3) 0.0023(3) 0.0302(12) Uani 1 1 d . . .
H34 H 0.2436 1.5931 -0.0290 0.036 Uiso 1 1 calc R . .
C35 C 0.2544(5) 1.4620(3) 0.0132(3) 0.0239(11) Uani 1 1 d . . .
C36 C 0.3844(5) 1.4264(3) -0.0213(3) 0.0227(11) Uani 1 1 d . . .
C37 C 0.4602(5) 1.4812(4) -0.0688(3) 0.0312(13) Uani 1 1 d . . .
H37 H 0.4278 1.5432 -0.0799 0.037 Uiso 1 1 calc R . .
C38 C 0.5823(6) 1.4458(4) -0.0998(3) 0.0352(14) Uani 1 1 d . . .
H38 H 0.6366 1.4825 -0.1310 0.042 Uiso 1 1 calc R . .
C39 C 0.6232(5) 1.3556(4) -0.0843(3) 0.0315(13) Uani 1 1 d . . .
H39 H 0.7067 1.3293 -0.1052 0.038 Uiso 1 1 calc R . .
C40 C 0.5433(5) 1.3025(3) -0.0381(3) 0.0241(11) Uani 1 1 d . . .
C41 C 0.5890(5) 1.2063(3) -0.0294(3) 0.0260(11) Uani 1 1 d . . .
C42 C 0.5299(5) 1.1646(4) -0.0582(3) 0.0287(12) Uani 1 1 d . . .
H42 H 0.4544 1.1953 -0.0788 0.034 Uiso 1 1 calc R . .
C43 C 0.5843(6) 1.0770(4) -0.0561(3) 0.0370(14) Uani 1 1 d . . .
H43 H 0.5475 1.0467 -0.0761 0.044 Uiso 1 1 calc R . .
C44 C 0.6922(6) 1.0345(4) -0.0248(3) 0.0431(16) Uani 1 1 d . . .
H44 H 0.7311 0.9744 -0.0227 0.052 Uiso 1 1 calc R . .
C45 C 0.7431(6) 1.0811(4) 0.0038(4) 0.0433(16) Uani 1 1 d . . .
H45 H 0.8163 1.0508 0.0266 0.052 Uiso 1 1 calc R . .
C46 C 0.5105(6) 1.3321(5) 0.2763(4) 0.0457(17) Uani 1 1 d . . .
C47 C 0.4208(5) 1.3099(3) 0.2450(3) 0.0257(11) Uani 1 1 d . A .
C48 C 0.3056(5) 1.2863(3) 0.2778(3) 0.0233(11) Uani 1 1 d . . .
H48 H 0.2660 1.2798 0.3259 0.028 Uiso 1 1 calc R A .
C49 C 0.2619(5) 1.2744(3) 0.2241(3) 0.0218(10) Uani 1 1 d . A .
C50 C 0.1478(5) 1.2507(3) 0.2181(2) 0.0197(10) Uani 1 1 d . . .
C51 C 0.0332(5) 1.2505(3) 0.2663(3) 0.0267(11) Uani 1 1 d . A .
H51 H 0.0256 1.2604 0.3111 0.032 Uiso 1 1 calc R . .
C52 C -0.0696(5) 1.2354(3) 0.2471(3) 0.0274(12) Uani 1 1 d . . .
H52 H -0.1489 1.2361 0.2793 0.033 Uiso 1 1 calc R A .
C53 C -0.0607(5) 1.2193(3) 0.1831(3) 0.0254(11) Uani 1 1 d . A .
H53 H -0.1317 1.2083 0.1710 0.030 Uiso 1 1 calc R . .
C54 C 0.0558(4) 1.2198(3) 0.1367(2) 0.0193(10) Uani 1 1 d . . .
C55 C 0.0833(5) 1.2127(3) 0.0646(2) 0.0195(10) Uani 1 1 d . A .
C56 C 0.0229(5) 1.1871(3) 0.0243(3) 0.0214(10) Uani 1 1 d . . .
H56 H -0.0540 1.1663 0.0382 0.026 Uiso 1 1 calc R A .
C57 C 0.1022(5) 1.1994(3) -0.0415(3) 0.0224(11) Uani 1 1 d . A .
C58 C 0.0841(6) 1.1841(4) -0.1057(3) 0.0334(13) Uani 1 1 d . . .
O2 O 0.4670(4) 1.0850(2) 0.1145(2) 0.0334(9) Uani 1 1 d . . .
F7 F 0.6257(7) 1.3355(7) 0.2364(4) 0.073(2) Uani 0.623(4) 1 d PU A 1
F8 F 0.4704(7) 1.4195(5) 0.2788(4) 0.072(2) Uani 0.623(4) 1 d PU A 1
F9 F 0.5197(10) 1.2899(6) 0.3416(5) 0.083(3) Uani 0.623(4) 1 d PU A 1
F10 F 0.0484(10) 1.1082(5) -0.0932(6) 0.066(3) Uani 0.623(4) 1 d PU A 1
F11 F 0.1858(9) 1.1838(7) -0.1564(4) 0.076(3) Uani 0.623(4) 1 d PU A 1
F12 F -0.0127(8) 1.2465(5) -0.1371(4) 0.071(2) Uani 0.623(4) 1 d PU A 1
F7' F 0.6073(11) 1.2565(10) 0.2969(8) 0.073(2) Uani 0.377(4) 1 d P A 2
F8' F 0.5686(15) 1.3878(9) 0.2380(9) 0.072(2) Uani 0.377(4) 1 d P A 2
F9' F 0.4547(16) 1.3441(11) 0.3395(8) 0.083(3) Uani 0.377(4) 1 d P A 2
F10' F -0.0058(18) 1.1449(10) -0.0954(10) 0.066(3) Uani 0.377(4) 1 d P A 2
F11' F 0.1899(16) 1.1258(11) -0.1306(7) 0.076(3) Uani 0.377(4) 1 d P A 2
F12' F 0.0829(15) 1.2494(9) -0.1605(7) 0.071(2) Uani 0.377(4) 1 d P A 2
O3 O 0.6899(5) 1.0012(4) 0.3558(3) 0.0792(18) Uani 1 1 d . . .
C59 C 0.6679(7) 1.0073(6) 0.2998(4) 0.058(2) Uani 1 1 d . . .
C60 C 0.6132(14) 0.9410(10) 0.2916(7) 0.175(7) Uani 1 1 d . . .
H60A H 0.5242 0.9674 0.2828 0.262 Uiso 1 1 calc R . .
H60B H 0.6137 0.8924 0.3349 0.262 Uiso 1 1 calc R . .
H60C H 0.6651 0.9186 0.2515 0.262 Uiso 1 1 calc R . .
C61 C 0.7060(18) 1.0673(9) 0.2355(7) 0.198(9) Uani 1 1 d . . .
H61A H 0.7667 1.0958 0.2427 0.297 Uiso 1 1 calc R . .
H61B H 0.6298 1.1119 0.2199 0.297 Uiso 1 1 calc R . .
H61C H 0.7480 1.0357 0.1992 0.297 Uiso 1 1 calc R . .
O4 O 0.4299(7) 1.3657(5) -0.2928(5) 0.133(3) Uani 1 1 d . . .
C62 C 0.5107(10) 1.3101(7) -0.2724(4) 0.073(3) Uani 1 1 d . . .
C63 C 0.4920(13) 1.2171(8) -0.2595(7) 0.142(5) Uani 1 1 d . . .
H63A H 0.5434 1.1925 -0.2985 0.212 Uiso 1 1 calc R . .
H63B H 0.4005 1.2201 -0.2569 0.212 Uiso 1 1 calc R . .
H63C H 0.5203 1.1796 -0.2148 0.212 Uiso 1 1 calc R . .
C64 C 0.6355(11) 1.3045(10) -0.2613(6) 0.146(6) Uani 1 1 d . . .
H64A H 0.6469 1.3638 -0.2692 0.219 Uiso 1 1 calc R . .
H64B H 0.7005 1.2754 -0.2944 0.219 Uiso 1 1 calc R . .
H64C H 0.6457 1.2705 -0.2125 0.219 Uiso 1 1 calc R . .
O5 O 0.3207(4) 0.8906(3) 0.3899(2) 0.0416(10) Uani 1 1 d . . .
H5A H 0.2476 0.8889 0.3843 0.062 Uiso 1 1 d R . .
H5B H 0.3513 0.8471 0.4212 0.062 Uiso 1 1 d R . .
O6 O 0.7029(3) 1.2705(3) 0.0937(2) 0.0344(9) Uani 1 1 d . . .
H6A H 0.7056 1.2366 0.0691 0.052 Uiso 1 1 d R . .
H6B H 0.6355 1.2740 0.1240 0.052 Uiso 1 1 d R . .
O7 O 0.2947(9) 1.3838(6) -0.1419(5) 0.164(4) Uani 1 1 d . . .
H7A H 0.3526 1.3756 -0.1862 0.247 Uiso 1 1 d R . .
H7B H 0.2726 1.3307 -0.1226 0.247 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C1 1.852(5) . ?
Os1 N6 2.020(4) . ?
Os1 N5 2.068(4) . ?
Os1 N7 2.072(4) . ?
Os1 N2 2.102(4) . ?
Os1 N1 2.133(4) . ?
N1 C2 1.337(6) . ?
N1 C6 1.349(6) . ?
N2 C11 1.362(6) . ?
N2 C7 1.375(6) . ?
N3 C12 1.334(6) . ?
N3 C16 1.346(7) . ?
N4 N5 1.343(5) . ?
N4 C18 1.356(6) . ?
N5 C20 1.371(6) . ?
N6 C25 1.358(6) . ?
N6 C21 1.363(6) . ?
N7 N8 1.341(5) . ?
N7 C26 1.368(6) . ?
N8 C28 1.352(6) . ?
C1 O1 1.152(6) . ?
C2 C3 1.376(7) . ?
C3 C4 1.373(8) . ?
C4 C5 1.373(7) . ?
C5 C6 1.392(7) . ?
C6 C7 1.479(7) . ?
C7 C8 1.383(7) . ?
C8 C9 1.372(7) . ?
C9 C10 1.379(7) . ?
C10 C11 1.390(6) . ?
C11 C12 1.482(7) . ?
C12 C13 1.390(7) . ?
C13 C14 1.370(7) . ?
C14 C15 1.380(8) . ?
C15 C16 1.378(8) . ?
C17 F1 1.332(6) . ?
C17 F2 1.339(6) . ?
C17 F3 1.341(6) . ?
C17 C18 1.479(7) . ?
C18 C19 1.380(7) . ?
C19 C20 1.388(7) . ?
C20 C21 1.457(7) . ?
C21 C22 1.391(7) . ?
C22 C23 1.379(7) . ?
C23 C24 1.390(7) . ?
C24 C25 1.372(7) . ?
C25 C26 1.465(7) . ?
C26 C27 1.382(7) . ?
C27 C28 1.388(7) . ?
C28 C29 1.481(7) . ?
C29 F6 1.319(7) . ?
C29 F5 1.326(7) . ?
C29 F4 1.330(7) . ?
Os2 C30 1.851(5) . ?
Os2 N14 2.022(4) . ?
Os2 N13 2.073(4) . ?
Os2 N15 2.082(4) . ?
Os2 N10 2.105(4) . ?
Os2 N9 2.134(4) . ?
N9 C31 1.347(6) . ?
N9 C35 1.352(6) . ?
N10 C40 1.351(6) . ?
N10 C36 1.371(6) . ?
N11 C45 1.331(7) . ?
N11 C41 1.342(7) . ?
N12 N13 1.349(5) . ?
N12 C47 1.350(6) . ?
N13 C49 1.363(6) . ?
N14 C50 1.353(6) . ?
N14 C54 1.358(6) . ?
N15 N16 1.342(5) . ?
N15 C55 1.374(6) . ?
N16 C57 1.337(6) . ?
C30 O2 1.158(6) . ?
C31 C32 1.381(7) . ?
C32 C33 1.363(8) . ?
C33 C34 1.378(8) . ?
C34 C35 1.385(7) . ?
C35 C36 1.468(7) . ?
C36 C37 1.390(7) . ?
C37 C38 1.377(8) . ?
C38 C39 1.377(8) . ?
C39 C40 1.392(7) . ?
C40 C41 1.485(7) . ?
C41 C42 1.390(7) . ?
C42 C43 1.383(8) . ?
C43 C44 1.373(9) . ?
C44 C45 1.389(9) . ?
C46 F8' 1.225(15) . ?
C46 F9 1.292(10) . ?
C46 F9' 1.325(18) . ?
C46 F7 1.331(10) . ?
C46 F8 1.393(10) . ?
C46 F7' 1.402(15) . ?
C46 C47 1.470(7) . ?
C47 C48 1.380(7) . ?
C48 C49 1.373(7) . ?
C49 C50 1.459(7) . ?
C50 C51 1.391(7) . ?
C51 C52 1.386(7) . ?
C52 C53 1.377(7) . ?
C53 C54 1.390(7) . ?
C54 C55 1.449(7) . ?
C55 C56 1.388(6) . ?
C56 C57 1.390(7) . ?
C57 C58 1.467(7) . ?
C58 F10' 1.273(19) . ?
C58 F12' 1.273(14) . ?
C58 F11 1.319(10) . ?
C58 F10 1.350(11) . ?
C58 F12 1.363(9) . ?
C58 F11' 1.378(17) . ?
O3 C59 1.181(9) . ?
C59 C61 1.414(13) . ?
C59 C60 1.461(12) . ?
O4 C62 1.120(10) . ?
C62 C64 1.413(13) . ?
C62 C63 1.539(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Os1 N6 91.20(18) . . ?
C1 Os1 N5 95.00(18) . . ?
N6 Os1 N5 78.25(16) . . ?
C1 Os1 N7 88.52(19) . . ?
N6 Os1 N7 78.32(16) . . ?
N5 Os1 N7 156.36(16) . . ?
C1 Os1 N2 101.15(17) . . ?
N6 Os1 N2 167.28(15) . . ?
N5 Os1 N2 103.43(15) . . ?
N7 Os1 N2 98.77(15) . . ?
C1 Os1 N1 177.18(18) . . ?
N6 Os1 N1 90.02(15) . . ?
N5 Os1 N1 87.74(15) . . ?
N7 Os1 N1 89.24(15) . . ?
N2 Os1 N1 77.50(15) . . ?
C2 N1 C6 118.9(4) . . ?
C2 N1 Os1 125.5(3) . . ?
C6 N1 Os1 115.5(3) . . ?
C11 N2 C7 116.6(4) . . ?
C11 N2 Os1 128.0(3) . . ?
C7 N2 Os1 115.0(3) . . ?
C12 N3 C16 117.3(5) . . ?
N5 N4 C18 105.2(4) . . ?
N4 N5 C20 110.2(4) . . ?
N4 N5 Os1 135.5(3) . . ?
C20 N5 Os1 114.4(3) . . ?
C25 N6 C21 121.9(4) . . ?
C25 N6 Os1 118.8(3) . . ?
C21 N6 Os1 118.8(3) . . ?
N8 N7 C26 109.8(4) . . ?
N8 N7 Os1 135.6(3) . . ?
C26 N7 Os1 114.3(3) . . ?
N7 N8 C28 106.0(4) . . ?
O1 C1 Os1 174.4(4) . . ?
N1 C2 C3 122.6(5) . . ?
C4 C3 C2 118.5(5) . . ?
C5 C4 C3 119.9(5) . . ?
C4 C5 C6 119.0(5) . . ?
N1 C6 C5 121.0(5) . . ?
N1 C6 C7 115.3(4) . . ?
C5 C6 C7 123.7(5) . . ?
N2 C7 C8 122.6(4) . . ?
N2 C7 C6 115.5(4) . . ?
C8 C7 C6 121.8(4) . . ?
C9 C8 C7 120.0(5) . . ?
C8 C9 C10 118.1(5) . . ?
C9 C10 C11 120.6(5) . . ?
N2 C11 C10 121.8(4) . . ?
N2 C11 C12 119.1(4) . . ?
C10 C11 C12 119.0(4) . . ?
N3 C12 C13 123.2(5) . . ?
N3 C12 C11 116.0(4) . . ?
C13 C12 C11 120.6(4) . . ?
C14 C13 C12 118.4(5) . . ?
C13 C14 C15 119.3(5) . . ?
C16 C15 C14 118.8(5) . . ?
N3 C16 C15 122.9(5) . . ?
F1 C17 F2 106.4(4) . . ?
F1 C17 F3 105.4(4) . . ?
F2 C17 F3 106.1(4) . . ?
F1 C17 C18 113.7(4) . . ?
F2 C17 C18 111.1(4) . . ?
F3 C17 C18 113.6(4) . . ?
N4 C18 C19 112.6(4) . . ?
N4 C18 C17 118.9(5) . . ?
C19 C18 C17 128.5(5) . . ?
C18 C19 C20 103.4(4) . . ?
N5 C20 C19 108.5(4) . . ?
N5 C20 C21 116.4(4) . . ?
C19 C20 C21 135.0(5) . . ?
N6 C21 C22 119.1(5) . . ?
N6 C21 C20 112.1(4) . . ?
C22 C21 C20 128.8(5) . . ?
C23 C22 C21 119.1(5) . . ?
C22 C23 C24 120.6(5) . . ?
C25 C24 C23 119.1(5) . . ?
N6 C25 C24 120.0(5) . . ?
N6 C25 C26 112.1(4) . . ?
C24 C25 C26 127.9(5) . . ?
N7 C26 C27 108.8(4) . . ?
N7 C26 C25 116.3(4) . . ?
C27 C26 C25 134.8(5) . . ?
C26 C27 C28 103.6(4) . . ?
N8 C28 C27 111.7(4) . . ?
N8 C28 C29 119.5(5) . . ?
C27 C28 C29 128.6(5) . . ?
F6 C29 F5 107.8(5) . . ?
F6 C29 F4 105.3(5) . . ?
F5 C29 F4 105.5(5) . . ?
F6 C29 C28 113.1(5) . . ?
F5 C29 C28 111.7(5) . . ?
F4 C29 C28 113.0(5) . . ?
C30 Os2 N14 93.12(18) . . ?
C30 Os2 N13 90.71(18) . . ?
N14 Os2 N13 78.26(15) . . ?
C30 Os2 N15 92.93(18) . . ?
N14 Os2 N15 78.38(15) . . ?
N13 Os2 N15 156.51(15) . . ?
C30 Os2 N10 101.19(18) . . ?
N14 Os2 N10 165.50(15) . . ?
N13 Os2 N10 99.03(15) . . ?
N15 Os2 N10 103.00(15) . . ?
C30 Os2 N9 176.72(18) . . ?
N14 Os2 N9 87.93(15) . . ?
N13 Os2 N9 86.46(15) . . ?
N15 Os2 N9 90.33(15) . . ?
N10 Os2 N9 77.65(15) . . ?
C31 N9 C35 118.4(4) . . ?
C31 N9 Os2 126.2(3) . . ?
C35 N9 Os2 115.0(3) . . ?
C40 N10 C36 117.4(4) . . ?
C40 N10 Os2 127.9(3) . . ?
C36 N10 Os2 114.5(3) . . ?
C45 N11 C41 117.1(5) . . ?
N13 N12 C47 105.1(4) . . ?
N12 N13 C49 109.8(4) . . ?
N12 N13 Os2 135.6(3) . . ?
C49 N13 Os2 114.4(3) . . ?
C50 N14 C54 121.9(4) . . ?
C50 N14 Os2 117.8(3) . . ?
C54 N14 Os2 118.2(3) . . ?
N16 N15 C55 110.1(4) . . ?
N16 N15 Os2 136.4(3) . . ?
C55 N15 Os2 113.3(3) . . ?
C57 N16 N15 105.8(4) . . ?
O2 C30 Os2 174.6(4) . . ?
N9 C31 C32 122.7(5) . . ?
C33 C32 C31 118.7(5) . . ?
C32 C33 C34 119.4(5) . . ?
C33 C34 C35 119.9(5) . . ?
N9 C35 C34 120.8(5) . . ?
N9 C35 C36 115.2(4) . . ?
C34 C35 C36 123.9(5) . . ?
N10 C36 C37 122.0(5) . . ?
N10 C36 C35 116.6(4) . . ?
C37 C36 C35 121.4(5) . . ?
C38 C37 C36 120.1(5) . . ?
C39 C38 C37 117.9(5) . . ?
C38 C39 C40 120.5(5) . . ?
N10 C40 C39 121.9(5) . . ?
N10 C40 C41 120.7(4) . . ?
C39 C40 C41 117.3(5) . . ?
N11 C41 C42 123.5(5) . . ?
N11 C41 C40 116.5(5) . . ?
C42 C41 C40 119.8(5) . . ?
C43 C42 C41 118.1(5) . . ?
C44 C43 C42 119.2(6) . . ?
C43 C44 C45 118.6(6) . . ?
N11 C45 C44 123.5(6) . . ?
F8' C46 F9 127.1(8) . . ?
F8' C46 F9' 115.0(11) . . ?
F9 C46 F9' 43.2(7) . . ?
F8' C46 F7 41.5(7) . . ?
F9 C46 F7 111.9(8) . . ?
F9' C46 F7 134.9(8) . . ?
F8' C46 F8 57.9(8) . . ?
F9 C46 F8 102.6(7) . . ?
F9' C46 F8 64.8(8) . . ?
F7 C46 F8 98.0(7) . . ?
F8' C46 F7' 104.9(10) . . ?
F9 C46 F7' 56.3(7) . . ?
F9' C46 F7' 99.2(9) . . ?
F7 C46 F7' 66.5(7) . . ?
F8 C46 F7' 140.0(7) . . ?
F8' C46 C47 116.9(8) . . ?
F9 C46 C47 116.0(6) . . ?
F9' C46 C47 110.1(8) . . ?
F7 C46 C47 114.9(6) . . ?
F8 C46 C47 111.1(6) . . ?
F7' C46 C47 108.9(7) . . ?
N12 C47 C48 112.5(4) . . ?
N12 C47 C46 119.4(5) . . ?
C48 C47 C46 128.0(5) . . ?
C49 C48 C47 103.4(4) . . ?
N13 C49 C48 109.2(4) . . ?
N13 C49 C50 115.6(4) . . ?
C48 C49 C50 135.2(5) . . ?
N14 C50 C51 119.8(4) . . ?
N14 C50 C49 112.9(4) . . ?
C51 C50 C49 127.0(5) . . ?
C52 C51 C50 118.1(5) . . ?
C53 C52 C51 122.2(5) . . ?
C52 C53 C54 117.7(5) . . ?
N14 C54 C53 120.4(4) . . ?
N14 C54 C55 112.2(4) . . ?
C53 C54 C55 127.2(4) . . ?
N15 C55 C56 108.2(4) . . ?
N15 C55 C54 116.7(4) . . ?
C56 C55 C54 135.0(4) . . ?
C55 C56 C57 103.2(4) . . ?
N16 C57 C56 112.7(4) . . ?
N16 C57 C58 120.0(5) . . ?
C56 C57 C58 127.3(5) . . ?
F10' C58 F12' 114.0(11) . . ?
F10' C58 F11 126.9(10) . . ?
F12' C58 F11 60.9(7) . . ?
F10' C58 F10 31.4(8) . . ?
F12' C58 F10 130.3(8) . . ?
F11 C58 F10 107.1(7) . . ?
F10' C58 F12 75.0(9) . . ?
F12' C58 F12 46.8(7) . . ?
F11 C58 F12 104.5(7) . . ?
F10 C58 F12 103.6(7) . . ?
F10' C58 F11' 101.6(10) . . ?
F12' C58 F11' 98.8(9) . . ?
F11 C58 F11' 40.1(7) . . ?
F10 C58 F11' 72.8(8) . . ?
F12 C58 F11' 132.8(8) . . ?
F10' C58 C57 113.7(10) . . ?
F12' C58 C57 115.4(7) . . ?
F11 C58 C57 114.6(6) . . ?
F10 C58 C57 113.1(6) . . ?
F12 C58 C57 112.9(5) . . ?
F11' C58 C57 111.3(8) . . ?
O3 C59 C61 125.6(9) . . ?
O3 C59 C60 119.3(9) . . ?
C61 C59 C60 114.4(10) . . ?
O4 C62 C64 134.3(11) . . ?
O4 C62 C63 115.7(10) . . ?
C64 C62 C63 109.6(11) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A N8 0.85 2.09 2.926(6) 170.9 .
O5 H5B N3 0.84 2.11 2.932(6) 167.9 .
O6 H6A N11 0.85 2.11 2.956(6) 172.6 .
O6 H6B N12 0.84 2.09 2.898(6) 163.4 .
O7 H7A O4 0.99 2.15 3.115(14) 164.5 .
O7 H7B N16 0.92 2.09 2.954(10) 156.5 .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.137

_database_code_depnum_ccdc_archive 'CCDC 989385'
