# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Tai-Chu Lau'
_publ_contact_author_email       bhtclau@cityu.edu.hk

_publ_section_title              
;
Binuclear (salen)osmium
phosphinidine and phosphiniminato complexes
;

# Attachment '- Os(salen)binuclear.Dalton(CIF).cif'

_publ_section_comment            
;
The unit cell contains two molecules of complexes. In each asymmetric unit,
there exist one molecules of the complex
[(methoxy)(imino-triphenylphosphine)(salchda)osmium(V)] perchlorate
monohydrate (salchda :<i>N,N</i>'-bis(salicylidene)<i>o</i>-cyclohexyldiamine).
The Os(V) atom is in a distorted octahedral geometry. The salchda act as
tetradentate ligand, coordinating through the two imino N and hydroxyl O
atoms. The Os---N and Os---O bond distances are within the normal range,
1.995(3)-2.005(3)\%A. The cyclohexyl ring still maintains its 'chair'
configuration. The chirality of the atoms C8 and C13 are both in
S-conformation.
In order to release the 5-membered diamine ring strain, the salchda ligand
is bent at one of the imine site, and the Os metal is raised 0.0204(15)\%A
from the O1/O2/N1/N2 plane. The dihedral angle between the salicylidene
rings O1/C1-C7 and O2/C14-C20 is 27.64(14)\%.

The imino-triphenylphosphine ligand is coordinated through the imino-N, where
Os---N distance is 2.026(3)\%A and N---P distance is 1.630(3)\%A, indicative
of single and double bonds respectively. The Os---O methoxy bond is
2.066(3)\%A showing the single bond character and no residual electron density
around the methoxy O atoms, signify that the methoxy group is deprotonated.

The perchlorate ion is disordered, it seems to rotate along the Cl1---O4 bond.
The occupancy ratio of the two disordered part is found to be about 0.573(12)
and 0.427(12). The water solvent molecule in the lattice seems to show very
vigorous thermal motion or display location flexibility, as shown by the big
thermal parameter. H-bonding with the main complex also observed, see H-bond
table.
;
_publ_section_references         
;
Bruker AXS Inc. (1998). <i>SMART</i> version 5.054, Madison, Wisconsin, USA.

Bruker AXS Inc. (1999). <i>SAINT</i>, version 6.02, Madison, Wisconsin, USA.

Johnson, C. K. (1976). <i>ORTEP</i>II, A FORTRAN Thermal-Ellipsoid Plot
Program, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge,
Tennessee, USA.

Rigaku/MSC and Rigaku Corporation. (2006). <i>CrystalStructure</i>. Single
Crystal Structure Analysis Software. Version 3.8.0. Rigaku/MSC, 9009 New
Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima,
Tokyo 196-8666, Japan.

Sheldrick, G. M. (1996). <i>SADABS</i>, G\"ottingen University, G\"ottingen,
Germany.

Sheldrick, G. M. (2008). <i>SHELXL97</i>, <i>SHELXS97</i> Acta Cryst. E68,
112-122.
;
_publ_section_acknowledgements   
;
(type here to add acknowledgements)
;

_publ_section_figure_captions    
;
Fig. 1. The <i>ORTEP</i> plot of the asymmetric unit was shown at 50%
probability thermal ellipsoids with the atom numbering scheme.
;
_publ_section_exptl_prep         
;
A red plate crystal of
[Os(C~20~H~20~N~2~O~2~){HN=P(C~6~H~5~)~3~}(OCH~3~)]^+^[ClO~4~]^-^.H~2~O having
approximate dimensions of 0.09mm <i>x</i> 0.12mm <i>x</i> 0.15mm was mounted
in glass capillary. All measurements were made on a Bruker <i>SMART</i> 1000
CCD area detector with graphite monochromated Mo---K\a radiation.

Indexing was performed from 60 images that were exposed for 10 s for a
preliminary unit cell determination. Of which, 88 out of total of 92
reflections were successfully indexed. The crystal-to-detector distance was
50.00 mm.

Cell constants and an orientation matrix for data collection corresponded to a
primitive triclinic cell with dimensions: a = 12.798(2)\%A, \a = 74.497(3)\%,
b = 13.354(2)\%A, \b = 63.096(2)\%, V = 1902.1(6)\%A^3^ c = 13.476(2)\%A, \g =
69.015(3)\%.

For <i>Z</i> = 2 and F.W. = 936.37, the calculated density is 1.635 g/cm^3^.
Based on a statistical analysis of intensity distribution, and the successful
solution and refinement of the structure, the space group was determined to
be: P -1 (#2)

The data were collected at a temperature of 25(1)\%C to a maximum 2\q value of
55.0\%. A total of 1421 oscillation images were collected in 4 runs. A sweep
of data was done using \w scans from 332.0 to 150.2\% in -0.3\% step, at
\c=54.7\% and \f = 0.0\%. The exposure rate was 30.0 [sec./\%]. The detector
swing angle was -28.00\%. A second sweep was performed using \w scans from
332.0 to 201.5\% in -0.3\% step, at \c=54.7\% and \f = 90.0\%. The exposure
rate was 30.0 [sec./\%]. The detector swing angle was -28.00\%. Another sweep
was performed using \w scans from 332.0 to 263\% in -0.3\% step, at \c=54.7\%
and \f = 180.0\%. The exposure rate was 30.0 [sec./\%]. A final sweep was
performed using \w scans from 332.0 to 317\% in -0.3\% step, at \c=54.7\% and
\f = 0.0\%. The exposure rate was 30.0 [sec./\%]. The crystal-to-detector
distance was 50.00 mm.

Of the 11671 reflections that was collected, 8180 reflections were unique.
(<i>R</i>~int~ = 0.0415); equivalent reflections were merged.
;
_publ_section_exptl_refinement   
;
The structure was solved by Direct methods (<i>SHELXS-97</i>) and expanded
using Fourier techniques. All non-H atoms were refined anisotropically.

All of the C-bound H atoms were observable from difference Fourier map but were
all placed at geometrical positions with C---H = 0.93, 0.96, 0.97 & 0.98\%A
for phenyl, methyl, methylene and methine H-atoms. The N- and O-bound H atoms
were located from difference Fourier syntheses map. All H-atoms were refined
using riding model with <i>U</i>~iso~(H) = 1.2<i>U</i>~eq~(Carrier). 25
restraints have been used in the refinement, 6 of which were related to
restraining similar aniostropic parameters of C39 with standard deviation of
0.002, while 18 of which were related to restraining similar aniostropic
parameters of O6, O7 and O7b with standard deviation of 0.01. One anti-bumping
restraint was also used in the refinement.
;
loop_
_publ_author_name
T.-C.Lau
W.-T.Wong

#==============================================================================
data_1b
_database_code_depnum_ccdc_archive 'CCDC 793797'
#TrackingRef '- Os(salen)binuclear.Dalton(CIF).cif'

# wt0575w-TCLau271-#3_1-6-2002

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H39 N3 O3 Os P, Cl O4, H2 O'
_chemical_formula_sum            'C39 H41 Cl N3 O8 Os P'
_chemical_formula_weight         936.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

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

_cell_length_a                   12.798(2)
_cell_length_b                   13.354(2)
_cell_length_c                   13.476(2)
_cell_angle_alpha                74.497(3)
_cell_angle_beta                 63.096(2)
_cell_angle_gamma                69.015(3)
_cell_volume                     1902.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    11671
_cell_measurement_theta_min      1.65
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    3.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6205
_exptl_absorpt_correction_T_max  0.7425
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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 1000 CCD Detector'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11671
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8180
_reflns_number_gt                6676
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'SMART (Bruker AXS Inc., 1998)'
_computing_cell_refinement       'SAINT (Bruker AXS Inc., 1999)'
_computing_data_reduction        
'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976) & Mercury'
_computing_publication_material  SHELXL-97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0460P)^2^] where P=(Fo^2^+2Fc^2^)/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         8180
_refine_ls_number_parameters     506
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0837
_refine_ls_wR_factor_gt          0.0788
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.985
_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
Os1 Os 0.524242(15) 0.293454(14) 0.373503(14) 0.03921(7) Uani 1 1 d . . .
P1 P 0.77318(10) 0.17712(9) 0.15911(9) 0.0378(2) Uani 1 1 d . . .
O1 O 0.5080(3) 0.1480(3) 0.3816(3) 0.0529(8) Uani 1 1 d . . .
O2 O 0.6468(3) 0.2289(2) 0.4433(2) 0.0431(7) Uani 1 1 d . . .
O3 O 0.3806(3) 0.3142(3) 0.5279(3) 0.0597(10) Uani 1 1 d . . .
O4 O 0.8056(4) 0.5675(4) -0.0952(3) 0.0896(14) Uani 1 1 d . . .
Cl1 Cl 0.70051(14) 0.57810(17) 0.00525(13) 0.0834(5) Uani 0.573(12) 1 d P A 1
O5 O 0.6774(11) 0.6939(9) 0.0300(10) 0.127(5) Uani 0.573(12) 1 d P A 1
O6 O 0.5958(12) 0.5949(14) -0.0140(12) 0.117(5) Uani 0.573(12) 1 d PU A 1
O7 O 0.7072(12) 0.5147(10) 0.0972(10) 0.098(4) Uani 0.573(12) 1 d PU A 1
Cl1B Cl 0.70051(14) 0.57810(17) 0.00525(13) 0.0834(5) Uani 0.427(12) 1 d P A 2
O5B O 0.6696(11) 0.4662(10) 0.0272(11) 0.107(6) Uani 0.427(12) 1 d P A 2
O6B O 0.7350(16) 0.5646(19) 0.0954(16) 0.114(7) Uani 0.427(12) 1 d P A 2
O7B O 0.6029(15) 0.6497(13) 0.0022(16) 0.104(7) Uani 0.427(12) 1 d PU A 2
O8 O 0.0822(15) 0.3875(15) 0.5340(11) 0.384(9) Uani 1 1 d . . .
H8A H 0.1309 0.3457 0.5550 0.460 Uiso 1 1 d . . .
H8B H 0.0599 0.4560 0.5403 0.460 Uiso 1 1 d . . .
N1 N 0.4075(3) 0.3697(3) 0.2984(3) 0.0412(8) Uani 1 1 d . . .
N2 N 0.5337(3) 0.4433(3) 0.3589(3) 0.0406(8) Uani 1 1 d . . .
N3 N 0.6662(3) 0.2782(3) 0.2222(3) 0.0412(8) Uani 1 1 d . . .
H1 H 0.6711 0.3396 0.1817 0.049 Uiso 1 1 calc R . .
C1 C 0.4330(4) 0.1294(4) 0.3508(4) 0.0480(11) Uani 1 1 d . . .
C2 C 0.4299(5) 0.0223(5) 0.3684(5) 0.0636(14) Uani 1 1 d . . .
H2 H 0.4785 -0.0312 0.4020 0.076 Uiso 1 1 calc R . .
C3 C 0.3571(6) -0.0052(5) 0.3374(5) 0.0749(17) Uani 1 1 d . . .
H3 H 0.3558 -0.0769 0.3514 0.090 Uiso 1 1 calc R . .
C4 C 0.2845(5) 0.0722(5) 0.2849(5) 0.0723(16) Uani 1 1 d . . .
H4 H 0.2373 0.0521 0.2619 0.087 Uiso 1 1 calc R . .
C5 C 0.2838(5) 0.1767(5) 0.2682(5) 0.0646(14) Uani 1 1 d . . .
H5 H 0.2344 0.2285 0.2344 0.078 Uiso 1 1 calc R . .
C6 C 0.3564(4) 0.2098(4) 0.3007(4) 0.0476(11) Uani 1 1 d . . .
C7 C 0.3488(4) 0.3230(4) 0.2763(4) 0.0482(11) Uani 1 1 d . . .
H7 H 0.2969 0.3670 0.2414 0.058 Uiso 1 1 calc R . .
C8 C 0.4006(4) 0.4867(4) 0.2617(4) 0.0462(10) Uani 1 1 d . . .
H8 H 0.4661 0.4931 0.1873 0.055 Uiso 1 1 calc R . .
C9 C 0.2812(5) 0.5583(4) 0.2533(5) 0.0628(14) Uani 1 1 d . . .
H9A H 0.2141 0.5538 0.3257 0.075 Uiso 1 1 calc R . .
H9B H 0.2667 0.5343 0.1999 0.075 Uiso 1 1 calc R . .
C10 C 0.2891(6) 0.6747(5) 0.2149(5) 0.0722(17) Uani 1 1 d . . .
H10A H 0.3520 0.6793 0.1398 0.087 Uiso 1 1 calc R . .
H10B H 0.2122 0.7212 0.2118 0.087 Uiso 1 1 calc R . .
C11 C 0.3176(6) 0.7150(4) 0.2928(5) 0.0710(16) Uani 1 1 d . . .
H11A H 0.2499 0.7190 0.3656 0.085 Uiso 1 1 calc R . .
H11B H 0.3271 0.7872 0.2626 0.085 Uiso 1 1 calc R . .
C12 C 0.4339(5) 0.6405(4) 0.3069(4) 0.0555(13) Uani 1 1 d . . .
H12A H 0.5036 0.6446 0.2364 0.067 Uiso 1 1 calc R . .
H12B H 0.4452 0.6640 0.3627 0.067 Uiso 1 1 calc R . .
C13 C 0.4262(4) 0.5263(4) 0.3426(4) 0.0470(11) Uani 1 1 d . . .
H13 H 0.3566 0.5255 0.4150 0.056 Uiso 1 1 calc R . .
C14 C 0.6235(4) 0.4655(4) 0.3596(4) 0.0449(10) Uani 1 1 d . . .
H14 H 0.6206 0.5380 0.3492 0.054 Uiso 1 1 calc R . .
C15 C 0.7277(4) 0.3862(4) 0.3751(4) 0.0463(11) Uani 1 1 d . . .
C16 C 0.8262(5) 0.4246(5) 0.3524(5) 0.0636(14) Uani 1 1 d . . .
H16 H 0.8191 0.4982 0.3325 0.076 Uiso 1 1 calc R . .
C17 C 0.9332(5) 0.3550(6) 0.3591(5) 0.0778(18) Uani 1 1 d . . .
H17 H 0.9998 0.3808 0.3381 0.093 Uiso 1 1 calc R . .
C18 C 0.9407(5) 0.2459(5) 0.3975(4) 0.0648(15) Uani 1 1 d . . .
H18 H 1.0120 0.1992 0.4042 0.078 Uiso 1 1 calc R . .
C19 C 0.8437(4) 0.2065(4) 0.4258(4) 0.0522(12) Uani 1 1 d . . .
H19 H 0.8503 0.1336 0.4524 0.063 Uiso 1 1 calc R . .
C20 C 0.7351(4) 0.2738(4) 0.4156(3) 0.0414(10) Uani 1 1 d . . .
C21 C 0.8488(4) 0.0730(3) 0.2418(4) 0.0418(10) Uani 1 1 d . . .
C22 C 0.7852(4) 0.0108(4) 0.3350(4) 0.0535(12) Uani 1 1 d . . .
H22 H 0.7010 0.0266 0.3606 0.064 Uiso 1 1 calc R . .
C23 C 0.8476(5) -0.0743(5) 0.3893(4) 0.0657(15) Uani 1 1 d . . .
H23 H 0.8047 -0.1156 0.4519 0.079 Uiso 1 1 calc R . .
C24 C 0.9717(5) -0.0992(5) 0.3528(5) 0.0673(15) Uani 1 1 d . . .
H24 H 1.0128 -0.1570 0.3900 0.081 Uiso 1 1 calc R . .
C25 C 1.0353(5) -0.0372(4) 0.2594(5) 0.0594(13) Uani 1 1 d . . .
H25 H 1.1195 -0.0531 0.2344 0.071 Uiso 1 1 calc R . .
C26 C 0.9751(4) 0.0470(4) 0.2042(4) 0.0499(11) Uani 1 1 d . . .
H26 H 1.0187 0.0873 0.1410 0.060 Uiso 1 1 calc R . .
C27 C 0.8868(4) 0.2360(4) 0.0468(4) 0.0423(10) Uani 1 1 d . . .
C28 C 0.9333(5) 0.3001(4) 0.0734(5) 0.0609(13) Uani 1 1 d . . .
H28 H 0.9041 0.3122 0.1474 0.073 Uiso 1 1 calc R . .
C29 C 1.0214(5) 0.3453(5) -0.0086(6) 0.0770(18) Uani 1 1 d . . .
H29 H 1.0531 0.3876 0.0092 0.092 Uiso 1 1 calc R . .
C30 C 1.0628(6) 0.3277(6) -0.1176(6) 0.089(2) Uani 1 1 d . . .
H30 H 1.1222 0.3592 -0.1736 0.106 Uiso 1 1 calc R . .
C31 C 1.0184(6) 0.2645(6) -0.1458(5) 0.083(2) Uani 1 1 d . . .
H31 H 1.0474 0.2539 -0.2202 0.100 Uiso 1 1 calc R . .
C32 C 0.9305(4) 0.2168(4) -0.0633(4) 0.0555(12) Uani 1 1 d . . .
H32 H 0.9012 0.1727 -0.0812 0.067 Uiso 1 1 calc R . .
C33 C 0.7179(4) 0.1075(4) 0.1030(4) 0.0407(10) Uani 1 1 d . . .
C34 C 0.7686(5) -0.0028(4) 0.0948(5) 0.0589(13) Uani 1 1 d . . .
H34 H 0.8294 -0.0422 0.1210 0.071 Uiso 1 1 calc R . .
C35 C 0.7277(5) -0.0537(5) 0.0473(5) 0.0715(16) Uani 1 1 d . . .
H35 H 0.7604 -0.1275 0.0424 0.086 Uiso 1 1 calc R . .
C36 C 0.6392(5) 0.0055(5) 0.0076(5) 0.0681(15) Uani 1 1 d . . .
H36 H 0.6137 -0.0280 -0.0264 0.082 Uiso 1 1 calc R . .
C37 C 0.5876(5) 0.1141(5) 0.0175(5) 0.0646(14) Uani 1 1 d . . .
H37 H 0.5259 0.1530 -0.0078 0.078 Uiso 1 1 calc R . .
C38 C 0.6270(4) 0.1659(4) 0.0649(4) 0.0503(11) Uani 1 1 d . . .
H38 H 0.5925 0.2394 0.0709 0.060 Uiso 1 1 calc R . .
C39 C 0.3748(6) 0.2506(6) 0.6004(6) 0.090(2) Uani 1 1 d U . .
H39A H 0.3034 0.2761 0.6648 0.108 Uiso 1 1 calc R . .
H39B H 0.4460 0.2330 0.6160 0.108 Uiso 1 1 calc R . .
H39C H 0.3702 0.1873 0.5835 0.108 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os1 0.03560(10) 0.04036(10) 0.04037(10) -0.01067(7) -0.01335(7) -0.00727(7)
P1 0.0337(5) 0.0383(6) 0.0400(6) -0.0124(5) -0.0141(5) -0.0036(5)
O1 0.0527(19) 0.0420(18) 0.067(2) -0.0018(15) -0.0292(17) -0.0130(15)
O2 0.0434(17) 0.0440(17) 0.0438(16) -0.0081(13) -0.0212(14) -0.0071(14)
O3 0.0490(19) 0.066(2) 0.051(2) -0.0369(18) -0.0260(17) 0.0277(18)
O4 0.060(2) 0.124(4) 0.069(3) -0.014(3) -0.014(2) -0.022(3)
Cl1 0.0555(8) 0.1209(15) 0.0643(9) -0.0098(9) -0.0203(7) -0.0196(9)
O5 0.124(9) 0.098(8) 0.154(10) -0.041(7) -0.047(7) -0.020(7)
O6 0.069(6) 0.185(14) 0.101(7) -0.023(9) -0.038(5) -0.030(9)
O7 0.092(8) 0.092(8) 0.069(6) 0.008(6) -0.028(6) 0.000(6)
Cl1B 0.0555(8) 0.1209(15) 0.0643(9) -0.0098(9) -0.0203(7) -0.0196(9)
O5B 0.093(9) 0.090(9) 0.106(10) -0.003(7) -0.009(7) -0.039(7)
O6B 0.092(10) 0.19(2) 0.073(9) -0.021(12) -0.026(7) -0.063(12)
O7B 0.070(9) 0.083(9) 0.106(10) -0.004(8) -0.032(7) 0.028(8)
O8 0.42(2) 0.42(2) 0.236(14) -0.073(13) -0.007(14) -0.179(18)
N1 0.0342(18) 0.043(2) 0.044(2) -0.0116(16) -0.0153(16) -0.0046(16)
N2 0.040(2) 0.039(2) 0.0407(19) -0.0111(15) -0.0163(16) -0.0038(16)
N3 0.044(2) 0.0329(18) 0.0394(19) -0.0093(15) -0.0145(16) -0.0026(16)
C1 0.039(2) 0.051(3) 0.051(3) -0.013(2) -0.007(2) -0.019(2)
C2 0.069(3) 0.055(3) 0.074(4) -0.010(3) -0.026(3) -0.026(3)
C3 0.082(4) 0.067(4) 0.093(4) -0.024(3) -0.029(4) -0.037(3)
C4 0.071(4) 0.089(5) 0.079(4) -0.022(3) -0.030(3) -0.039(4)
C5 0.060(3) 0.077(4) 0.072(4) -0.015(3) -0.030(3) -0.026(3)
C6 0.038(2) 0.056(3) 0.052(3) -0.017(2) -0.013(2) -0.013(2)
C7 0.038(2) 0.055(3) 0.052(3) -0.013(2) -0.016(2) -0.010(2)
C8 0.048(3) 0.038(2) 0.052(3) -0.010(2) -0.023(2) -0.004(2)
C9 0.062(3) 0.051(3) 0.076(4) -0.014(3) -0.040(3) 0.005(3)
C10 0.084(4) 0.054(3) 0.079(4) -0.015(3) -0.051(3) 0.009(3)
C11 0.088(4) 0.045(3) 0.082(4) -0.024(3) -0.047(3) 0.008(3)
C12 0.065(3) 0.042(3) 0.058(3) -0.020(2) -0.030(3) 0.003(2)
C13 0.048(3) 0.045(3) 0.045(2) -0.015(2) -0.019(2) -0.002(2)
C14 0.047(3) 0.038(2) 0.050(3) -0.0104(19) -0.019(2) -0.009(2)
C15 0.045(3) 0.054(3) 0.043(2) -0.013(2) -0.016(2) -0.015(2)
C16 0.057(3) 0.066(4) 0.075(4) -0.008(3) -0.026(3) -0.026(3)
C17 0.051(3) 0.099(5) 0.093(5) -0.010(4) -0.031(3) -0.029(3)
C18 0.047(3) 0.088(4) 0.064(3) -0.018(3) -0.029(3) -0.009(3)
C19 0.048(3) 0.057(3) 0.051(3) -0.017(2) -0.023(2) -0.003(2)
C20 0.042(2) 0.049(3) 0.032(2) -0.0125(18) -0.0135(18) -0.007(2)
C21 0.042(2) 0.039(2) 0.045(2) -0.0150(19) -0.021(2) 0.0002(19)
C22 0.046(3) 0.053(3) 0.047(3) -0.008(2) -0.013(2) -0.003(2)
C23 0.069(4) 0.055(3) 0.051(3) 0.000(2) -0.019(3) -0.004(3)
C24 0.076(4) 0.053(3) 0.069(4) -0.010(3) -0.043(3) 0.008(3)
C25 0.050(3) 0.059(3) 0.073(3) -0.020(3) -0.035(3) 0.003(3)
C26 0.045(3) 0.049(3) 0.058(3) -0.012(2) -0.023(2) -0.008(2)
C27 0.033(2) 0.043(2) 0.044(2) -0.0084(19) -0.0128(19) -0.0038(19)
C28 0.050(3) 0.057(3) 0.072(3) -0.018(3) -0.013(3) -0.017(3)
C29 0.054(3) 0.059(4) 0.106(5) -0.016(3) -0.018(3) -0.017(3)
C30 0.064(4) 0.069(4) 0.090(5) 0.009(4) -0.003(4) -0.022(3)
C31 0.077(4) 0.087(5) 0.051(3) 0.000(3) -0.009(3) -0.013(4)
C32 0.049(3) 0.060(3) 0.046(3) -0.009(2) -0.014(2) -0.008(2)
C33 0.033(2) 0.043(2) 0.046(2) -0.0163(19) -0.0123(18) -0.0078(19)
C34 0.050(3) 0.051(3) 0.082(4) -0.026(3) -0.032(3) 0.000(2)
C35 0.058(3) 0.061(3) 0.105(5) -0.043(3) -0.034(3) -0.001(3)
C36 0.058(3) 0.079(4) 0.087(4) -0.032(3) -0.030(3) -0.024(3)
C37 0.053(3) 0.074(4) 0.076(4) -0.019(3) -0.031(3) -0.013(3)
C38 0.049(3) 0.047(3) 0.058(3) -0.009(2) -0.026(2) -0.009(2)
C39 0.067(3) 0.088(4) 0.105(4) -0.046(3) -0.004(3) -0.024(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 O1 1.995(3) . ?
Os1 N2 1.999(4) . ?
Os1 O2 2.005(3) . ?
Os1 N1 2.006(3) . ?
Os1 N3 2.026(3) . ?
Os1 O3 2.066(3) . ?
P1 N3 1.630(3) . ?
P1 C27 1.793(4) . ?
P1 C33 1.808(4) . ?
P1 C21 1.816(4) . ?
O1 C1 1.321(6) . ?
O2 C20 1.326(5) . ?
O3 C39 1.104(7) . ?
O4 Cl1 1.407(4) . ?
Cl1 O7 1.320(12) . ?
Cl1 O6 1.408(13) . ?
Cl1 O5 1.564(11) . ?
O8 H8A 0.7789 . ?
O8 H8B 0.8706 . ?
N1 C7 1.295(6) . ?
N1 C8 1.489(6) . ?
N2 C14 1.290(6) . ?
N2 C13 1.490(5) . ?
N3 H1 0.8600 . ?
C1 C2 1.397(7) . ?
C1 C6 1.423(7) . ?
C2 C3 1.363(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.395(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.350(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.420(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.435(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.521(6) . ?
C8 C13 1.528(6) . ?
C8 H8 0.9800 . ?
C9 C10 1.527(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.521(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.528(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.497(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13 0.9800 . ?
C14 C15 1.437(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.405(7) . ?
C15 C20 1.438(7) . ?
C16 C17 1.379(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.394(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.377(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.404(6) . ?
C19 H19 0.9300 . ?
C21 C22 1.389(6) . ?
C21 C26 1.393(6) . ?
C22 C23 1.378(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.369(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.390(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.365(7) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C32 1.389(6) . ?
C27 C28 1.393(7) . ?
C28 C29 1.364(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.374(10) . ?
C29 H29 0.9300 . ?
C30 C31 1.374(11) . ?
C30 H30 0.9300 . ?
C31 C32 1.381(8) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C38 1.379(6) . ?
C33 C34 1.393(7) . ?
C34 C35 1.392(7) . ?
C34 H34 0.9300 . ?
C35 C36 1.369(8) . ?
C35 H35 0.9300 . ?
C36 C37 1.377(8) . ?
C36 H36 0.9300 . ?
C37 C38 1.384(7) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Os1 N2 176.04(13) . . ?
O1 Os1 O2 91.45(13) . . ?
N2 Os1 O2 92.46(13) . . ?
O1 Os1 N1 93.41(14) . . ?
N2 Os1 N1 82.66(15) . . ?
O2 Os1 N1 174.83(13) . . ?
O1 Os1 N3 91.69(14) . . ?
N2 Os1 N3 87.84(14) . . ?
O2 Os1 N3 87.53(13) . . ?
N1 Os1 N3 90.55(14) . . ?
O1 Os1 O3 90.43(15) . . ?
N2 Os1 O3 90.07(15) . . ?
O2 Os1 O3 92.17(12) . . ?
N1 Os1 O3 89.57(13) . . ?
N3 Os1 O3 177.87(15) . . ?
N3 P1 C27 105.3(2) . . ?
N3 P1 C33 111.96(19) . . ?
C27 P1 C33 109.7(2) . . ?
N3 P1 C21 116.89(19) . . ?
C27 P1 C21 107.1(2) . . ?
C33 P1 C21 105.7(2) . . ?
C1 O1 Os1 125.3(3) . . ?
C20 O2 Os1 120.4(3) . . ?
C39 O3 Os1 121.8(4) . . ?
O7 Cl1 O4 118.7(6) . . ?
O7 Cl1 O6 116.9(9) . . ?
O4 Cl1 O6 111.2(6) . . ?
O7 Cl1 O5 104.0(7) . . ?
O4 Cl1 O5 103.0(5) . . ?
O6 Cl1 O5 99.5(8) . . ?
H8A O8 H8B 122.0 . . ?
C7 N1 C8 122.0(4) . . ?
C7 N1 Os1 124.7(3) . . ?
C8 N1 Os1 113.1(3) . . ?
C14 N2 C13 124.1(4) . . ?
C14 N2 Os1 124.3(3) . . ?
C13 N2 Os1 111.5(3) . . ?
P1 N3 Os1 135.0(2) . . ?
P1 N3 H1 112.5 . . ?
Os1 N3 H1 112.5 . . ?
O1 C1 C2 117.0(5) . . ?
O1 C1 C6 124.8(4) . . ?
C2 C1 C6 118.2(5) . . ?
C3 C2 C1 121.2(6) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 121.2(6) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 119.1(5) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 121.9(6) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 118.4(5) . . ?
C5 C6 C7 116.3(5) . . ?
C1 C6 C7 125.3(4) . . ?
N1 C7 C6 126.2(4) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
N1 C8 C9 115.4(4) . . ?
N1 C8 C13 107.7(3) . . ?
C9 C8 C13 110.3(4) . . ?
N1 C8 H8 107.7 . . ?
C9 C8 H8 107.7 . . ?
C13 C8 H8 107.7 . . ?
C8 C9 C10 108.8(5) . . ?
C8 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
C8 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C11 C10 C9 112.2(5) . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C10 C11 C12 111.5(4) . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C13 C12 C11 110.4(5) . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
N2 C13 C12 116.9(4) . . ?
N2 C13 C8 106.7(3) . . ?
C12 C13 C8 112.2(4) . . ?
N2 C13 H13 106.8 . . ?
C12 C13 H13 106.8 . . ?
C8 C13 H13 106.8 . . ?
N2 C14 C15 124.7(4) . . ?
N2 C14 H14 117.6 . . ?
C15 C14 H14 117.6 . . ?
C16 C15 C14 116.2(5) . . ?
C16 C15 C20 119.1(4) . . ?
C14 C15 C20 124.7(4) . . ?
C17 C16 C15 121.2(5) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 119.5(5) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 120.7(5) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C20 121.5(5) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
O2 C20 C19 117.6(4) . . ?
O2 C20 C15 124.6(4) . . ?
C19 C20 C15 117.8(4) . . ?
C22 C21 C26 119.2(4) . . ?
C22 C21 P1 121.3(3) . . ?
C26 C21 P1 119.2(4) . . ?
C23 C22 C21 119.6(5) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C24 C23 C22 121.2(5) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C23 C24 C25 119.2(5) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C26 C25 C24 120.5(5) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 120.4(5) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C32 C27 C28 120.3(5) . . ?
C32 C27 P1 121.9(4) . . ?
C28 C27 P1 117.8(4) . . ?
C29 C28 C27 120.2(6) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C28 C29 C30 119.3(7) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
C29 C30 C31 121.5(6) . . ?
C29 C30 H30 119.3 . . ?
C31 C30 H30 119.3 . . ?
C30 C31 C32 119.8(6) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C31 C32 C27 118.9(6) . . ?
C31 C32 H32 120.5 . . ?
C27 C32 H32 120.5 . . ?
C38 C33 C34 120.2(4) . . ?
C38 C33 P1 119.0(3) . . ?
C34 C33 P1 120.8(4) . . ?
C35 C34 C33 119.7(5) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C36 C35 C34 119.6(5) . . ?
C36 C35 H35 120.2 . . ?
C34 C35 H35 120.2 . . ?
C35 C36 C37 120.6(5) . . ?
C35 C36 H36 119.7 . . ?
C37 C36 H36 119.7 . . ?
C36 C37 C38 120.5(5) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C33 C38 C37 119.4(5) . . ?
C33 C38 H38 120.3 . . ?
C37 C38 H38 120.3 . . ?
O3 C39 H39A 109.5 . . ?
O3 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O3 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H1 O5B 0.86 2.31 3.107(13) 154.8 .
N3 H1 O7 0.86 2.42 3.260(13) 165.8 .
O8 H8B O8 0.87 2.55 3.17(4) 129.1 2_566

_diffrn_measured_fraction_theta_max 0.936
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.936
_refine_diff_density_max         1.900
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.106

# start Validation Reply Form
_vrf_PLAT029_wt0575w-shelxl      
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.94
RESPONSE: A standard data collection routine was used which supposedly
should have covered the hemisphere data. May be due to the orientation
of the crystal, some of the reflections were not covered for triclinic
primitive space group, thus the fraction of measured data is less than
95%.
;
# end Validation Reply Form

data_2
_database_code_depnum_ccdc_archive 'CCDC 793798'
#TrackingRef '- Os(salen)binuclear.Dalton(CIF).cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H40 F6 N5 O2 Os P2'
_chemical_formula_weight         1012.93

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   11.4181(2)
_cell_length_b                   19.5201(4)
_cell_length_c                   18.4402(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.891(2)
_cell_angle_gamma                90.00
_cell_volume                     3971.98(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8905
_cell_measurement_theta_min      3.5777
_cell_measurement_theta_max      28.0414

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2012
_exptl_absorpt_coefficient_mu    3.364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro, Oxford Diffraction Ltd'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.1270
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14759
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.59
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6976
_reflns_number_gt                5223
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep-3
_computing_publication_material  Wingx

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         6976
_refine_ls_number_parameters     507
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0603
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      0.954
_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
Os1 Os 0.173809(14) 0.235222(9) 0.497017(9) 0.01841(6) Uani 1 1 d . B .
P1 P 0.36951(9) 0.23436(6) 0.38928(6) 0.0195(2) Uani 1 1 d . B .
P2A P 0.88640(13) 0.04763(8) 0.19922(8) 0.0461(4) Uiso 0.531(11) 1 d P A 1
F1A F 0.8329(6) 0.0337(4) 0.2715(4) 0.049(2) Uiso 0.531(11) 1 d P A 1
F2A F 0.9428(8) 0.0637(5) 0.1289(4) 0.065(3) Uiso 0.531(11) 1 d P A 1
F3A F 1.0166(6) 0.0702(4) 0.2465(4) 0.053(2) Uiso 0.531(11) 1 d P A 1
F4A F 0.9247(10) -0.0227(5) 0.1874(6) 0.092(3) Uiso 0.531(11) 1 d P A 1
F5A F 0.7528(6) 0.0353(4) 0.1445(3) 0.058(2) Uiso 0.531(11) 1 d P A 1
F6A F 0.8411(8) 0.1267(5) 0.2040(4) 0.076(3) Uiso 0.531(11) 1 d P A 1
P2B P 0.88640(13) 0.04763(8) 0.19922(8) 0.0461(4) Uiso 0.469(11) 1 d P A 2
F1B F 0.8548(7) 0.0121(4) 0.2696(4) 0.041(2) Uiso 0.469(11) 1 d P A 2
F2B F 0.9130(8) 0.0829(5) 0.1290(4) 0.048(2) Uiso 0.469(11) 1 d P A 2
F3B F 0.9869(6) 0.0890(4) 0.2611(4) 0.040(2) Uiso 0.469(11) 1 d P A 2
F4B F 0.9811(10) -0.0187(5) 0.2103(6) 0.078(3) Uiso 0.469(11) 1 d P A 2
F5B F 0.7891(7) -0.0024(5) 0.1463(4) 0.052(3) Uiso 0.469(11) 1 d P A 2
F6B F 0.7937(11) 0.1032(6) 0.1954(6) 0.094(4) Uiso 0.469(11) 1 d P A 2
O1 O 0.2730(2) 0.14733(14) 0.52129(15) 0.0216(6) Uani 1 1 d . . .
O2 O 0.3133(2) 0.28920(15) 0.56077(15) 0.0247(7) Uani 1 1 d . . .
N1 N 0.0294(3) 0.18655(18) 0.43516(17) 0.0208(8) Uani 1 1 d . . .
N2 N 0.0733(3) 0.31831(19) 0.46487(19) 0.0257(8) Uani 1 1 d . . .
N3 N 0.2403(3) 0.24994(17) 0.40529(18) 0.0238(9) Uani 1 1 d . . .
H3N H 0.1877 0.2685 0.3669 0.029 Uiso 1 1 calc R B .
N4 N 0.1140(3) 0.22342(17) 0.59371(17) 0.0205(8) Uani 1 1 d . . .
N5 N 0.0564(4) 0.2095(2) 0.7317(2) 0.0403(10) Uani 1 1 d . B .
C1 C 0.2323(4) 0.0867(2) 0.4972(2) 0.0234(10) Uani 1 1 d . B .
C2 C 0.3138(4) 0.0310(2) 0.5168(2) 0.0302(11) Uani 1 1 d . . .
H2A H 0.3943 0.0395 0.5455 0.036 Uiso 1 1 calc R . .
C3 C 0.2804(5) -0.0343(3) 0.4957(3) 0.0407(12) Uani 1 1 d . . .
H3A H 0.3373 -0.0704 0.5104 0.049 Uiso 1 1 calc R . .
C4 C 0.1646(5) -0.0491(2) 0.4531(3) 0.0436(13) Uani 1 1 d . . .
H4A H 0.1420 -0.0948 0.4384 0.052 Uiso 1 1 calc R . .
C5 C 0.0833(4) 0.0030(2) 0.4327(3) 0.0365(12) Uani 1 1 d . B .
H5A H 0.0038 -0.0075 0.4036 0.044 Uiso 1 1 calc R . .
C6 C 0.1120(4) 0.0716(2) 0.4528(2) 0.0254(10) Uani 1 1 d . . .
C7 C 0.0203(4) 0.1211(2) 0.4245(2) 0.0262(10) Uani 1 1 d . B .
H7A H -0.0551 0.1044 0.3949 0.031 Uiso 1 1 calc R . .
C8A C -0.0567(7) 0.2345(4) 0.3852(5) 0.0196(19) Uiso 0.55 1 d PD B 1
H8AA H -0.0270 0.2455 0.3400 0.023 Uiso 0.55 1 calc PR B 1
C9A C -0.1874(8) 0.2103(5) 0.3609(6) 0.031(3) Uiso 0.55 1 d PD B 1
H9AA H -0.2227 0.2082 0.4046 0.037 Uiso 0.55 1 calc PR B 1
H9AB H -0.1919 0.1641 0.3383 0.037 Uiso 0.55 1 calc PR B 1
C10A C -0.2579(9) 0.2633(5) 0.3020(6) 0.038(3) Uiso 0.55 1 d PD B 1
H10A H -0.2174 0.2693 0.2610 0.045 Uiso 0.55 1 calc PR B 1
H10B H -0.3420 0.2476 0.2801 0.045 Uiso 0.55 1 calc PR B 1
C11A C -0.2572(8) 0.3306(5) 0.3447(6) 0.041(3) Uiso 0.55 1 d PD B 1
H11A H -0.2955 0.3235 0.3866 0.049 Uiso 0.55 1 calc PR B 1
H11B H -0.3048 0.3656 0.3106 0.049 Uiso 0.55 1 calc PR B 1
C12A C -0.1268(10) 0.3559(6) 0.3757(7) 0.028(4) Uiso 0.55 1 d PD B 1
H12A H -0.1265 0.4005 0.4014 0.034 Uiso 0.55 1 calc PR B 1
H12B H -0.0870 0.3620 0.3344 0.034 Uiso 0.55 1 calc PR B 1
C13A C -0.0585(7) 0.3011(4) 0.4320(4) 0.0192(18) Uiso 0.55 1 d PD B 1
H13A H -0.1005 0.2928 0.4726 0.023 Uiso 0.55 1 calc PR B 1
C8B C -0.0763(10) 0.2333(6) 0.4091(7) 0.036(3) Uiso 0.45 1 d PD B 2
H8BA H -0.1140 0.2351 0.4524 0.044 Uiso 0.45 1 calc PR B 2
C9B C -0.1784(10) 0.2072(6) 0.3436(7) 0.028(4) Uiso 0.45 1 d PD B 2
H9BA H -0.1464 0.1975 0.2996 0.033 Uiso 0.45 1 calc PR B 2
H9BB H -0.2128 0.1643 0.3581 0.033 Uiso 0.45 1 calc PR B 2
C10B C -0.2764(11) 0.2622(6) 0.3240(8) 0.044(4) Uiso 0.45 1 d PD B 2
H10C H -0.3315 0.2497 0.2749 0.053 Uiso 0.45 1 calc PR B 2
H10D H -0.3244 0.2594 0.3616 0.053 Uiso 0.45 1 calc PR B 2
C11B C -0.2418(12) 0.3344(6) 0.3192(8) 0.053(4) Uiso 0.45 1 d PD B 2
H11C H -0.3133 0.3639 0.3166 0.063 Uiso 0.45 1 calc PR B 2
H11D H -0.2155 0.3414 0.2726 0.063 Uiso 0.45 1 calc PR B 2
C12B C -0.1384(13) 0.3560(8) 0.3874(9) 0.040(6) Uiso 0.45 1 d PD B 2
H12C H -0.1072 0.4015 0.3777 0.048 Uiso 0.45 1 calc PR B 2
H12D H -0.1702 0.3598 0.4324 0.048 Uiso 0.45 1 calc PR B 2
C13B C -0.0369(10) 0.3046(5) 0.4017(7) 0.041(3) Uiso 0.45 1 d PD B 2
H13B H -0.0071 0.3049 0.3552 0.049 Uiso 0.45 1 calc PR B 2
C14 C 0.1113(4) 0.3806(2) 0.4763(2) 0.0281(10) Uani 1 1 d . B .
H14A H 0.0565 0.4160 0.4542 0.034 Uiso 1 1 calc R . .
C15 C 0.2290(4) 0.4008(2) 0.5193(3) 0.0317(11) Uani 1 1 d . . .
C16 C 0.2526(5) 0.4723(3) 0.5236(3) 0.0549(16) Uani 1 1 d . B .
H16A H 0.1917 0.5030 0.4975 0.066 Uiso 1 1 calc R . .
C17 C 0.3593(6) 0.4975(3) 0.5639(4) 0.077(2) Uani 1 1 d . . .
H17A H 0.3727 0.5456 0.5664 0.092 Uiso 1 1 calc R B .
C18 C 0.4484(6) 0.4540(3) 0.6011(3) 0.0616(17) Uani 1 1 d . B .
H18A H 0.5244 0.4723 0.6277 0.074 Uiso 1 1 calc R . .
C19 C 0.4307(4) 0.3847(3) 0.6009(3) 0.0384(12) Uani 1 1 d . . .
H19A H 0.4931 0.3558 0.6288 0.046 Uiso 1 1 calc R B .
C20 C 0.3210(4) 0.3560(2) 0.5598(2) 0.0273(10) Uani 1 1 d . B .
C21 C 0.4979(4) 0.2452(2) 0.4682(2) 0.0235(10) Uani 1 1 d . . .
C22 C 0.5635(4) 0.3052(2) 0.4807(3) 0.0354(12) Uani 1 1 d . B .
H22A H 0.5382 0.3429 0.4478 0.042 Uiso 1 1 calc R . .
C23 C 0.6656(4) 0.3119(3) 0.5400(3) 0.0449(13) Uani 1 1 d . . .
H23A H 0.7098 0.3536 0.5474 0.054 Uiso 1 1 calc R B .
C24 C 0.7025(5) 0.2583(3) 0.5878(3) 0.0454(14) Uani 1 1 d . B .
H24A H 0.7732 0.2627 0.6281 0.054 Uiso 1 1 calc R . .
C25 C 0.6383(4) 0.1981(3) 0.5783(3) 0.0399(13) Uani 1 1 d . . .
H25A H 0.6636 0.1614 0.6125 0.048 Uiso 1 1 calc R B .
C26 C 0.5361(4) 0.1909(2) 0.5186(2) 0.0307(11) Uani 1 1 d . B .
H26A H 0.4921 0.1491 0.5118 0.037 Uiso 1 1 calc R . .
C27 C 0.3830(4) 0.1497(2) 0.3546(2) 0.0222(9) Uani 1 1 d . . .
C28 C 0.4952(4) 0.1248(2) 0.3487(2) 0.0298(11) Uani 1 1 d . B .
H28A H 0.5667 0.1508 0.3682 0.036 Uiso 1 1 calc R . .
C29 C 0.5020(4) 0.0623(2) 0.3146(3) 0.0390(12) Uani 1 1 d . . .
H29A H 0.5777 0.0458 0.3095 0.047 Uiso 1 1 calc R B .
C30 C 0.3989(5) 0.0247(3) 0.2882(3) 0.0454(14) Uani 1 1 d . B .
H30A H 0.4040 -0.0184 0.2653 0.054 Uiso 1 1 calc R . .
C31 C 0.2875(4) 0.0481(3) 0.2940(3) 0.0434(13) Uani 1 1 d . . .
H31A H 0.2168 0.0212 0.2753 0.052 Uiso 1 1 calc R B .
C32 C 0.2796(4) 0.1107(2) 0.3272(2) 0.0299(11) Uani 1 1 d . B .
H32A H 0.2033 0.1271 0.3313 0.036 Uiso 1 1 calc R . .
C33 C 0.3827(3) 0.2925(2) 0.3164(2) 0.0201(9) Uani 1 1 d . . .
C34 C 0.4053(3) 0.2702(2) 0.2498(2) 0.0225(9) Uani 1 1 d . B .
H34A H 0.4177 0.2228 0.2426 0.027 Uiso 1 1 calc R . .
C35 C 0.4100(4) 0.3163(3) 0.1941(2) 0.0312(11) Uani 1 1 d . . .
H35A H 0.4257 0.3008 0.1487 0.037 Uiso 1 1 calc R B .
C36 C 0.3920(4) 0.3846(3) 0.2043(2) 0.0346(12) Uani 1 1 d . B .
H36A H 0.3953 0.4163 0.1657 0.042 Uiso 1 1 calc R . .
C37 C 0.3693(4) 0.4078(2) 0.2698(3) 0.0323(11) Uani 1 1 d . . .
H37A H 0.3586 0.4554 0.2767 0.039 Uiso 1 1 calc R B .
C38 C 0.3621(4) 0.3619(2) 0.3252(2) 0.0280(10) Uani 1 1 d . B .
H38A H 0.3431 0.3777 0.3696 0.034 Uiso 1 1 calc R . .
C39 C 0.0968(4) 0.2779(2) 0.6344(2) 0.0288(11) Uani 1 1 d . B .
H39A H 0.1048 0.3227 0.6161 0.035 Uiso 1 1 calc R . .
C40 C 0.0681(4) 0.2704(3) 0.7015(3) 0.0370(12) Uani 1 1 d . . .
H40A H 0.0560 0.3105 0.7278 0.044 Uiso 1 1 calc R B .
C41 C 0.0725(4) 0.1556(3) 0.6915(3) 0.0337(11) Uani 1 1 d . . .
H41A H 0.0649 0.1109 0.7103 0.040 Uiso 1 1 calc R B .
C42 C 0.1001(4) 0.1624(2) 0.6232(2) 0.0274(10) Uani 1 1 d . B .
H42A H 0.1095 0.1222 0.5962 0.033 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os1 0.01889(9) 0.01771(9) 0.01897(9) -0.00024(8) 0.00549(6) 0.00197(8)
P1 0.0187(5) 0.0200(5) 0.0201(5) 0.0017(5) 0.0054(4) 0.0006(5)
O1 0.0226(15) 0.0182(17) 0.0215(15) -0.0037(13) 0.0014(12) 0.0040(13)
O2 0.0269(15) 0.0202(16) 0.0251(16) -0.0015(13) 0.0030(13) -0.0016(14)
N1 0.0150(17) 0.029(2) 0.0173(18) 0.0039(16) 0.0020(14) 0.0046(16)
N2 0.025(2) 0.027(2) 0.0242(19) 0.0004(17) 0.0048(16) 0.0087(17)
N3 0.0213(17) 0.035(2) 0.0165(17) 0.0079(15) 0.0082(14) 0.0058(16)
N4 0.0188(17) 0.024(2) 0.0182(17) -0.0002(15) 0.0042(14) 0.0074(15)
N5 0.046(2) 0.047(3) 0.030(2) 0.003(2) 0.0152(19) 0.012(2)
C1 0.028(2) 0.022(3) 0.020(2) 0.000(2) 0.0059(18) 0.001(2)
C2 0.030(2) 0.031(3) 0.026(3) -0.005(2) 0.000(2) 0.011(2)
C3 0.046(3) 0.027(3) 0.042(3) -0.004(2) -0.004(2) 0.010(2)
C4 0.051(3) 0.021(3) 0.051(3) -0.010(2) -0.001(3) 0.000(3)
C5 0.037(3) 0.023(3) 0.044(3) -0.006(2) 0.000(2) -0.002(2)
C6 0.025(2) 0.026(3) 0.025(2) 0.000(2) 0.0051(19) 0.002(2)
C7 0.021(2) 0.032(3) 0.025(2) -0.004(2) 0.0041(19) -0.004(2)
C14 0.035(3) 0.022(3) 0.028(2) 0.003(2) 0.009(2) 0.009(2)
C15 0.040(3) 0.022(3) 0.031(3) 0.004(2) 0.006(2) 0.002(2)
C16 0.072(4) 0.021(3) 0.064(4) 0.005(3) 0.004(3) -0.004(3)
C17 0.087(5) 0.030(3) 0.096(5) 0.001(4) -0.008(4) -0.021(4)
C18 0.067(4) 0.034(3) 0.068(4) -0.006(3) -0.009(3) -0.026(3)
C19 0.046(3) 0.034(3) 0.034(3) -0.005(2) 0.008(2) -0.010(3)
C20 0.038(3) 0.026(3) 0.022(2) -0.006(2) 0.015(2) -0.001(2)
C21 0.019(2) 0.032(3) 0.020(2) -0.0023(19) 0.0067(17) 0.005(2)
C22 0.038(3) 0.034(3) 0.029(3) -0.001(2) -0.001(2) -0.003(2)
C23 0.042(3) 0.046(4) 0.040(3) -0.012(3) -0.001(2) -0.011(3)
C24 0.035(3) 0.064(4) 0.030(3) -0.012(3) -0.004(2) 0.000(3)
C25 0.033(3) 0.051(4) 0.031(3) 0.005(2) -0.001(2) 0.008(3)
C26 0.027(2) 0.033(3) 0.030(3) 0.003(2) 0.005(2) 0.005(2)
C27 0.026(2) 0.020(2) 0.020(2) 0.0044(18) 0.0039(18) 0.003(2)
C28 0.024(2) 0.025(3) 0.039(3) 0.003(2) 0.005(2) 0.001(2)
C29 0.035(3) 0.032(3) 0.049(3) -0.007(2) 0.008(2) 0.013(2)
C30 0.050(3) 0.029(3) 0.051(3) -0.016(3) 0.003(3) 0.005(3)
C31 0.037(3) 0.034(3) 0.053(3) -0.009(3) 0.002(3) -0.004(3)
C32 0.027(2) 0.032(3) 0.029(2) 0.001(2) 0.003(2) -0.001(2)
C33 0.0151(19) 0.022(2) 0.022(2) 0.0017(19) 0.0024(17) 0.0007(19)
C34 0.0154(19) 0.025(2) 0.025(2) -0.001(2) 0.0010(17) 0.0002(19)
C35 0.029(2) 0.044(3) 0.019(2) 0.000(2) 0.0034(19) -0.005(2)
C36 0.037(3) 0.038(3) 0.026(3) 0.009(2) 0.002(2) -0.009(2)
C37 0.037(3) 0.022(3) 0.035(3) 0.002(2) 0.005(2) -0.005(2)
C38 0.026(2) 0.034(3) 0.024(2) -0.002(2) 0.0063(19) -0.002(2)
C39 0.031(2) 0.026(3) 0.032(3) -0.002(2) 0.013(2) 0.005(2)
C40 0.040(3) 0.040(3) 0.030(3) -0.009(2) 0.009(2) 0.010(3)
C41 0.037(3) 0.034(3) 0.033(3) 0.002(2) 0.013(2) 0.002(2)
C42 0.031(2) 0.027(3) 0.028(2) -0.002(2) 0.014(2) 0.000(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
Os1 N2 1.987(3) . ?
Os1 N1 1.989(3) . ?
Os1 O2 2.016(3) . ?
Os1 O1 2.041(3) . ?
Os1 N3 2.045(3) . ?
Os1 N4 2.079(3) . ?
P1 N3 1.606(3) . ?
P1 C27 1.793(4) . ?
P1 C21 1.793(4) . ?
P1 C33 1.795(4) . ?
P2A F4A 1.473(9) . ?
P2A F3A 1.581(6) . ?
P2A F5A 1.616(6) . ?
P2A F2A 1.620(8) . ?
P2A F1A 1.626(7) . ?
P2A F6A 1.637(8) . ?
O1 C1 1.306(5) . ?
O2 C20 1.307(5) . ?
N1 C7 1.293(5) . ?
N1 C8B 1.490(12) . ?
N1 C8A 1.492(9) . ?
N2 C14 1.290(5) . ?
N2 C13B 1.503(11) . ?
N2 C13A 1.509(8) . ?
N3 H3N 0.8800 . ?
N4 C42 1.336(5) . ?
N4 C39 1.345(5) . ?
N5 C41 1.328(6) . ?
N5 C40 1.335(6) . ?
C1 C2 1.417(6) . ?
C1 C6 1.437(6) . ?
C2 C3 1.359(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.383(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.363(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.405(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.422(6) . ?
C7 H7A 0.9500 . ?
C8A C9A 1.520(11) . ?
C8A C13A 1.564(10) . ?
C8A H8AA 1.0000 . ?
C9A C10A 1.565(11) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
C10A C11A 1.530(12) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
C11A C12A 1.534(12) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C12A C13A 1.554(11) . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C13A H13A 1.0000 . ?
C8B C13B 1.480(13) . ?
C8B C9B 1.534(13) . ?
C8B H8BA 1.0000 . ?
C9B C10B 1.525(13) . ?
C9B H9BA 0.9900 . ?
C9B H9BB 0.9900 . ?
C10B C11B 1.473(14) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
C11B C12B 1.545(14) . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C12B C13B 1.504(14) . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
C13B H13B 1.0000 . ?
C14 C15 1.429(6) . ?
C14 H14A 0.9500 . ?
C15 C16 1.420(7) . ?
C15 C20 1.423(6) . ?
C16 C17 1.347(8) . ?
C16 H16A 0.9500 . ?
C17 C18 1.367(8) . ?
C17 H17A 0.9500 . ?
C18 C19 1.367(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.403(6) . ?
C19 H19A 0.9500 . ?
C21 C22 1.378(6) . ?
C21 C26 1.402(6) . ?
C22 C23 1.385(6) . ?
C22 H22A 0.9500 . ?
C23 C24 1.362(7) . ?
C23 H23A 0.9500 . ?
C24 C25 1.372(7) . ?
C24 H24A 0.9500 . ?
C25 C26 1.390(6) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 C32 1.386(6) . ?
C27 C28 1.400(6) . ?
C28 C29 1.383(6) . ?
C28 H28A 0.9500 . ?
C29 C30 1.367(7) . ?
C29 H29A 0.9500 . ?
C30 C31 1.382(7) . ?
C30 H30A 0.9500 . ?
C31 C32 1.381(6) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
C33 C34 1.388(5) . ?
C33 C38 1.393(6) . ?
C34 C35 1.377(6) . ?
C34 H34A 0.9500 . ?
C35 C36 1.369(6) . ?
C35 H35A 0.9500 . ?
C36 C37 1.375(6) . ?
C36 H36A 0.9500 . ?
C37 C38 1.378(6) . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9500 . ?
C39 C40 1.365(6) . ?
C39 H39A 0.9500 . ?
C40 H40A 0.9500 . ?
C41 C42 1.380(6) . ?
C41 H41A 0.9500 . ?
C42 H42A 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
N2 Os1 N1 83.60(14) . . ?
N2 Os1 O2 93.24(13) . . ?
N1 Os1 O2 176.44(12) . . ?
N2 Os1 O1 175.40(12) . . ?
N1 Os1 O1 93.19(12) . . ?
O2 Os1 O1 90.06(11) . . ?
N2 Os1 N3 86.99(13) . . ?
N1 Os1 N3 91.27(13) . . ?
O2 Os1 N3 90.20(12) . . ?
O1 Os1 N3 89.80(12) . . ?
N2 Os1 N4 93.12(13) . . ?
N1 Os1 N4 91.85(13) . . ?
O2 Os1 N4 86.67(12) . . ?
O1 Os1 N4 90.27(11) . . ?
N3 Os1 N4 176.87(13) . . ?
N3 P1 C27 114.03(19) . . ?
N3 P1 C21 115.22(18) . . ?
C27 P1 C21 105.71(19) . . ?
N3 P1 C33 106.02(18) . . ?
C27 P1 C33 106.50(19) . . ?
C21 P1 C33 108.99(19) . . ?
F4A P2A F3A 93.9(5) . . ?
F4A P2A F5A 92.1(4) . . ?
F3A P2A F5A 171.5(4) . . ?
F4A P2A F2A 82.4(5) . . ?
F3A P2A F2A 82.9(4) . . ?
F5A P2A F2A 92.0(4) . . ?
F4A P2A F1A 98.8(5) . . ?
F3A P2A F1A 95.3(4) . . ?
F5A P2A F1A 89.6(3) . . ?
F2A P2A F1A 177.9(4) . . ?
F4A P2A F6A 174.7(5) . . ?
F3A P2A F6A 88.5(4) . . ?
F5A P2A F6A 85.0(4) . . ?
F2A P2A F6A 93.2(4) . . ?
F1A P2A F6A 85.6(4) . . ?
C1 O1 Os1 123.9(2) . . ?
C20 O2 Os1 124.0(3) . . ?
C7 N1 C8B 122.0(5) . . ?
C7 N1 C8A 120.8(4) . . ?
C8B N1 C8A 21.0(5) . . ?
C7 N1 Os1 125.5(3) . . ?
C8B N1 Os1 112.1(5) . . ?
C8A N1 Os1 111.8(4) . . ?
C14 N2 C13B 118.3(5) . . ?
C14 N2 C13A 122.3(4) . . ?
C13B N2 C13A 25.7(5) . . ?
C14 N2 Os1 125.2(3) . . ?
C13B N2 Os1 113.0(4) . . ?
C13A N2 Os1 112.2(3) . . ?
P1 N3 Os1 132.79(19) . . ?
P1 N3 H3N 113.6 . . ?
Os1 N3 H3N 113.6 . . ?
C42 N4 C39 115.3(4) . . ?
C42 N4 Os1 123.2(3) . . ?
C39 N4 Os1 121.2(3) . . ?
C41 N5 C40 115.4(4) . . ?
O1 C1 C2 117.1(4) . . ?
O1 C1 C6 125.7(4) . . ?
C2 C1 C6 117.1(4) . . ?
C3 C2 C1 122.0(4) . . ?
C3 C2 H2A 119.0 . . ?
C1 C2 H2A 119.0 . . ?
C2 C3 C4 121.0(5) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C5 C4 C3 119.0(4) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
C4 C5 C6 122.7(4) . . ?
C4 C5 H5A 118.6 . . ?
C6 C5 H5A 118.6 . . ?
C5 C6 C7 116.7(4) . . ?
C5 C6 C1 118.1(4) . . ?
C7 C6 C1 125.1(4) . . ?
N1 C7 C6 126.4(4) . . ?
N1 C7 H7A 116.8 . . ?
C6 C7 H7A 116.8 . . ?
N1 C8A C9A 115.3(7) . . ?
N1 C8A C13A 106.3(6) . . ?
C9A C8A C13A 105.6(7) . . ?
N1 C8A H8AA 109.8 . . ?
C9A C8A H8AA 109.8 . . ?
C13A C8A H8AA 109.8 . . ?
C8A C9A C10A 106.8(8) . . ?
C8A C9A H9AA 110.4 . . ?
C10A C9A H9AA 110.4 . . ?
C8A C9A H9AB 110.4 . . ?
C10A C9A H9AB 110.4 . . ?
H9AA C9A H9AB 108.6 . . ?
C11A C10A C9A 106.1(8) . . ?
C11A C10A H10A 110.5 . . ?
C9A C10A H10A 110.5 . . ?
C11A C10A H10B 110.5 . . ?
C9A C10A H10B 110.5 . . ?
H10A C10A H10B 108.7 . . ?
C10A C11A C12A 110.1(9) . . ?
C10A C11A H11A 109.6 . . ?
C12A C11A H11A 109.6 . . ?
C10A C11A H11B 109.6 . . ?
C12A C11A H11B 109.6 . . ?
H11A C11A H11B 108.1 . . ?
C11A C12A C13A 107.4(8) . . ?
C11A C12A H12A 110.2 . . ?
C13A C12A H12A 110.2 . . ?
C11A C12A H12B 110.2 . . ?
C13A C12A H12B 110.2 . . ?
H12A C12A H12B 108.5 . . ?
N2 C13A C12A 113.1(7) . . ?
N2 C13A C8A 104.6(5) . . ?
C12A C13A C8A 106.2(7) . . ?
N2 C13A H13A 110.9 . . ?
C12A C13A H13A 110.9 . . ?
C8A C13A H13A 110.9 . . ?
C13B C8B N1 111.5(8) . . ?
C13B C8B C9B 115.3(10) . . ?
N1 C8B C9B 116.0(9) . . ?
C13B C8B H8BA 104.1 . . ?
N1 C8B H8BA 104.1 . . ?
C9B C8B H8BA 104.1 . . ?
C10B C9B C8B 108.4(10) . . ?
C10B C9B H9BA 110.0 . . ?
C8B C9B H9BA 110.0 . . ?
C10B C9B H9BB 110.0 . . ?
C8B C9B H9BB 110.0 . . ?
H9BA C9B H9BB 108.4 . . ?
C11B C10B C9B 119.8(11) . . ?
C11B C10B H10C 107.4 . . ?
C9B C10B H10C 107.4 . . ?
C11B C10B H10D 107.4 . . ?
C9B C10B H10D 107.4 . . ?
H10C C10B H10D 106.9 . . ?
C10B C11B C12B 111.9(12) . . ?
C10B C11B H11C 109.2 . . ?
C12B C11B H11C 109.2 . . ?
C10B C11B H11D 109.2 . . ?
C12B C11B H11D 109.2 . . ?
H11C C11B H11D 107.9 . . ?
C13B C12B C11B 110.7(11) . . ?
C13B C12B H12C 109.5 . . ?
C11B C12B H12C 109.5 . . ?
C13B C12B H12D 109.5 . . ?
C11B C12B H12D 109.5 . . ?
H12C C12B H12D 108.1 . . ?
C8B C13B N2 108.1(8) . . ?
C8B C13B C12B 113.9(11) . . ?
N2 C13B C12B 118.1(9) . . ?
C8B C13B H13B 105.2 . . ?
N2 C13B H13B 105.2 . . ?
C12B C13B H13B 105.2 . . ?
N2 C14 C15 125.4(4) . . ?
N2 C14 H14A 117.3 . . ?
C15 C14 H14A 117.3 . . ?
C16 C15 C20 118.1(4) . . ?
C16 C15 C14 116.1(4) . . ?
C20 C15 C14 125.8(4) . . ?
C17 C16 C15 121.4(5) . . ?
C17 C16 H16A 119.3 . . ?
C15 C16 H16A 119.3 . . ?
C16 C17 C18 120.1(6) . . ?
C16 C17 H17A 120.0 . . ?
C18 C17 H17A 120.0 . . ?
C19 C18 C17 121.5(5) . . ?
C19 C18 H18A 119.2 . . ?
C17 C18 H18A 119.2 . . ?
C18 C19 C20 120.5(5) . . ?
C18 C19 H19A 119.7 . . ?
C20 C19 H19A 119.7 . . ?
O2 C20 C19 116.5(4) . . ?
O2 C20 C15 125.2(4) . . ?
C19 C20 C15 118.3(4) . . ?
C22 C21 C26 118.0(4) . . ?
C22 C21 P1 122.1(3) . . ?
C26 C21 P1 119.9(3) . . ?
C21 C22 C23 121.5(5) . . ?
C21 C22 H22A 119.2 . . ?
C23 C22 H22A 119.2 . . ?
C24 C23 C22 119.8(5) . . ?
C24 C23 H23A 120.1 . . ?
C22 C23 H23A 120.1 . . ?
C23 C24 C25 120.5(5) . . ?
C23 C24 H24A 119.7 . . ?
C25 C24 H24A 119.7 . . ?
C24 C25 C26 120.0(5) . . ?
C24 C25 H25A 120.0 . . ?
C26 C25 H25A 120.0 . . ?
C25 C26 C21 120.2(4) . . ?
C25 C26 H26A 119.9 . . ?
C21 C26 H26A 119.9 . . ?
C32 C27 C28 119.4(4) . . ?
C32 C27 P1 119.5(3) . . ?
C28 C27 P1 120.8(3) . . ?
C29 C28 C27 120.1(4) . . ?
C29 C28 H28A 120.0 . . ?
C27 C28 H28A 120.0 . . ?
C30 C29 C28 119.5(4) . . ?
C30 C29 H29A 120.3 . . ?
C28 C29 H29A 120.3 . . ?
C29 C30 C31 121.3(5) . . ?
C29 C30 H30A 119.3 . . ?
C31 C30 H30A 119.3 . . ?
C32 C31 C30 119.6(5) . . ?
C32 C31 H31A 120.2 . . ?
C30 C31 H31A 120.2 . . ?
C31 C32 C27 120.1(4) . . ?
C31 C32 H32A 120.0 . . ?
C27 C32 H32A 120.0 . . ?
C34 C33 C38 119.0(4) . . ?
C34 C33 P1 122.4(3) . . ?
C38 C33 P1 118.6(3) . . ?
C35 C34 C33 120.4(4) . . ?
C35 C34 H34A 119.8 . . ?
C33 C34 H34A 119.8 . . ?
C36 C35 C34 119.9(4) . . ?
C36 C35 H35A 120.0 . . ?
C34 C35 H35A 120.0 . . ?
C35 C36 C37 120.7(4) . . ?
C35 C36 H36A 119.7 . . ?
C37 C36 H36A 119.7 . . ?
C36 C37 C38 119.8(4) . . ?
C36 C37 H37A 120.1 . . ?
C38 C37 H37A 120.1 . . ?
C37 C38 C33 120.1(4) . . ?
C37 C38 H38A 119.9 . . ?
C33 C38 H38A 119.9 . . ?
N4 C39 C40 121.6(4) . . ?
N4 C39 H39A 119.2 . . ?
C40 C39 H39A 119.2 . . ?
N5 C40 C39 123.2(4) . . ?
N5 C40 H40A 118.4 . . ?
C39 C40 H40A 118.4 . . ?
N5 C41 C42 122.0(4) . . ?
N5 C41 H41A 119.0 . . ?
C42 C41 H41A 119.0 . . ?
N4 C42 C41 122.5(4) . . ?
N4 C42 H42A 118.8 . . ?
C41 C42 H42A 118.8 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.466
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.098

data_3
_database_code_depnum_ccdc_archive 'CCDC 793799'
#TrackingRef '- Os(salen)binuclear.Dalton(CIF).cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C77.50 H75 Cl3 F12 N6 O5 Os2 P4'
_chemical_formula_weight         2009.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -4.9801 6.2216 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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'

_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                   14.2178(3)
_cell_length_b                   14.9520(3)
_cell_length_c                   20.6258(5)
_cell_angle_alpha                69.1705(19)
_cell_angle_beta                 84.0361(17)
_cell_angle_gamma                68.1080(18)
_cell_volume                     3800.56(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    16942
_cell_measurement_theta_min      3.3741
_cell_measurement_theta_max      71.4359

_exptl_crystal_description       block
_exptl_crystal_colour            'dark purple'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1986
_exptl_absorpt_coefficient_mu    8.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.17800
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro, Oxford Diffraction Ltd'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.1270
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24719
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         66.99
_reflns_number_total             13369
_reflns_number_gt                10683
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep-3
_computing_publication_material  Wingx

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0893P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         13369
_refine_ls_number_parameters     985
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1215
_refine_ls_wR_factor_gt          0.1162
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.111818(16) 0.139646(17) 0.756521(10) 0.01372(8) Uani 1 1 d . . .
Os2 Os 0.388359(16) 0.032855(16) 0.761471(10) 0.01369(8) Uani 1 1 d . . .
P1 P -0.11894(10) 0.30679(11) 0.70200(7) 0.0170(3) Uani 1 1 d . . .
P2 P 0.61969(11) -0.08446(11) 0.71792(7) 0.0178(3) Uani 1 1 d . . .
P3 P 0.24458(13) 0.63300(13) 0.70202(8) 0.0279(3) Uani 1 1 d . . .
P4 P 0.75008(11) 0.04729(11) 0.87293(7) 0.0202(3) Uani 1 1 d . . .
F1 F 0.2449(5) 0.5387(5) 0.6837(3) 0.0764(18) Uani 1 1 d . . .
F2 F 0.1739(4) 0.6097(5) 0.7657(3) 0.0684(17) Uani 1 1 d . . .
F3 F 0.1450(4) 0.7054(5) 0.6521(3) 0.0600(14) Uani 1 1 d . . .
F4 F 0.2432(5) 0.7296(4) 0.7183(3) 0.0630(15) Uani 1 1 d . . .
F5 F 0.3422(4) 0.5638(4) 0.7504(3) 0.0639(15) Uani 1 1 d . . .
F6 F 0.3135(4) 0.6593(4) 0.6374(2) 0.0511(12) Uani 1 1 d . . .
F7 F 0.6673(3) -0.0037(3) 0.8756(2) 0.0335(9) Uani 1 1 d . . .
F8 F 0.8098(4) 0.0022(4) 0.8153(3) 0.0587(14) Uani 1 1 d . . .
F9 F 0.8152(4) -0.0531(4) 0.9325(3) 0.0569(14) Uani 1 1 d . . .
F10 F 0.6905(4) 0.0932(4) 0.9304(3) 0.0530(13) Uani 1 1 d . . .
F11 F 0.6847(4) 0.1480(4) 0.8142(3) 0.0621(15) Uani 1 1 d . . .
F12 F 0.8340(3) 0.0977(3) 0.8717(2) 0.0326(8) Uani 1 1 d . . .
O1 O 0.1030(3) 0.1964(3) 0.65098(19) 0.0229(9) Uani 1 1 d . . .
O2 O 0.1175(3) 0.2723(3) 0.75703(19) 0.0175(8) Uani 1 1 d . . .
O3 O 0.3857(3) -0.1082(3) 0.77910(19) 0.0177(8) Uani 1 1 d . . .
O4 O 0.3912(3) 0.0606(3) 0.65736(19) 0.0198(8) Uani 1 1 d . . .
O5 O 0.2497(3) 0.0853(3) 0.75803(17) 0.0186(8) Uani 1 1 d . . .
N1 N 0.1022(3) 0.0072(4) 0.7614(2) 0.0143(9) Uani 1 1 d . . .
N2 N 0.1110(4) 0.0775(4) 0.8612(2) 0.0205(10) Uani 1 1 d . . .
N3 N 0.3918(3) 0.0148(4) 0.8626(2) 0.0139(9) Uani 1 1 d . . .
N4 N 0.3915(3) 0.1713(3) 0.7492(2) 0.0145(9) Uani 1 1 d . . .
N5 N -0.0416(4) 0.2061(4) 0.7581(2) 0.0204(10) Uani 1 1 d . . .
H5N H -0.0700 0.1754 0.7948 0.024 Uiso 1 1 calc R . .
N6 N 0.5432(4) -0.0338(4) 0.7703(2) 0.0194(10) Uani 1 1 d . . .
H6N H 0.5718 -0.0352 0.8067 0.023 Uiso 1 1 calc R . .
C1 C 0.1099(4) 0.1402(5) 0.6123(3) 0.0184(11) Uani 1 1 d . . .
C2 C 0.1063(5) 0.1908(5) 0.5400(3) 0.0263(13) Uani 1 1 d . . .
H2A H 0.1017 0.2603 0.5223 0.032 Uiso 1 1 calc R . .
C3 C 0.1093(6) 0.1418(6) 0.4948(3) 0.0404(18) Uani 1 1 d . . .
H3A H 0.1072 0.1774 0.4462 0.048 Uiso 1 1 calc R . .
C4 C 0.1153(7) 0.0400(6) 0.5190(4) 0.047(2) Uani 1 1 d . . .
H4A H 0.1159 0.0070 0.4871 0.057 Uiso 1 1 calc R . .
C5 C 0.1204(6) -0.0123(5) 0.5893(4) 0.0366(17) Uani 1 1 d . . .
H5A H 0.1274 -0.0825 0.6056 0.044 Uiso 1 1 calc R . .
C6 C 0.1153(5) 0.0372(5) 0.6382(3) 0.0261(13) Uani 1 1 d . . .
C7 C 0.1110(4) -0.0240(5) 0.7092(3) 0.0210(12) Uani 1 1 d . . .
H7A H 0.1149 -0.0923 0.7186 0.025 Uiso 1 1 calc R . .
C8 C 0.0850(5) -0.0577(4) 0.8319(3) 0.0198(12) Uani 1 1 d . . .
H8A H 0.0104 -0.0337 0.8394 0.024 Uiso 1 1 calc R . .
C9 C 0.1221(5) -0.1709(5) 0.8470(3) 0.0255(13) Uani 1 1 d . . .
H9A H 0.1962 -0.1969 0.8408 0.031 Uiso 1 1 calc R . .
H9B H 0.0891 -0.1853 0.8138 0.031 Uiso 1 1 calc R . .
C10 C 0.0989(6) -0.2262(5) 0.9205(3) 0.0333(15) Uani 1 1 d . . .
H10A H 0.1281 -0.3012 0.9302 0.040 Uiso 1 1 calc R . .
H10B H 0.0245 -0.2061 0.9251 0.040 Uiso 1 1 calc R . .
C11 C 0.1423(5) -0.2007(5) 0.9731(3) 0.0284(14) Uani 1 1 d . . .
H11A H 0.2173 -0.2317 0.9739 0.034 Uiso 1 1 calc R . .
H11B H 0.1194 -0.2318 1.0198 0.034 Uiso 1 1 calc R . .
C12 C 0.1108(5) -0.0854(5) 0.9572(3) 0.0251(13) Uani 1 1 d . . .
H12A H 0.1465 -0.0733 0.9901 0.030 Uiso 1 1 calc R . .
H12B H 0.0370 -0.0555 0.9633 0.030 Uiso 1 1 calc R . .
C13 C 0.1362(5) -0.0327(4) 0.8829(3) 0.0192(12) Uani 1 1 d . . .
H13A H 0.2112 -0.0644 0.8789 0.023 Uiso 1 1 calc R . .
C14 C 0.1004(4) 0.1287(4) 0.9028(3) 0.0178(11) Uani 1 1 d . . .
H14A H 0.0982 0.0934 0.9510 0.021 Uiso 1 1 calc R . .
C15 C 0.0916(4) 0.2342(5) 0.8818(3) 0.0198(12) Uani 1 1 d . . .
C16 C 0.0785(5) 0.2728(5) 0.9373(3) 0.0235(12) Uani 1 1 d . . .
H16A H 0.0730 0.2299 0.9831 0.028 Uiso 1 1 calc R . .
C17 C 0.0737(5) 0.3702(5) 0.9263(4) 0.0316(14) Uani 1 1 d . . .
H17A H 0.0632 0.3955 0.9637 0.038 Uiso 1 1 calc R . .
C18 C 0.0847(5) 0.4321(5) 0.8585(4) 0.0297(14) Uani 1 1 d . . .
H18A H 0.0818 0.4997 0.8505 0.036 Uiso 1 1 calc R . .
C19 C 0.0992(5) 0.3979(5) 0.8048(3) 0.0231(12) Uani 1 1 d . . .
H19A H 0.1075 0.4415 0.7598 0.028 Uiso 1 1 calc R . .
C20 C 0.1023(4) 0.2984(5) 0.8136(3) 0.0196(11) Uani 1 1 d . . .
C21 C 0.4059(4) -0.1821(5) 0.8406(3) 0.0224(12) Uani 1 1 d . . .
C22 C 0.4117(5) -0.2786(5) 0.8428(3) 0.0220(12) Uani 1 1 d . . .
H22A H 0.4029 -0.2878 0.8009 0.026 Uiso 1 1 calc R . .
C23 C 0.4296(5) -0.3603(5) 0.9037(3) 0.0228(12) Uani 1 1 d . . .
H23A H 0.4332 -0.4249 0.9035 0.027 Uiso 1 1 calc R . .
C24 C 0.4428(5) -0.3484(5) 0.9667(3) 0.0258(13) Uani 1 1 d . . .
H24A H 0.4562 -0.4050 1.0090 0.031 Uiso 1 1 calc R . .
C25 C 0.4363(5) -0.2551(5) 0.9661(3) 0.0234(12) Uani 1 1 d . . .
H25A H 0.4441 -0.2475 1.0088 0.028 Uiso 1 1 calc R . .
C26 C 0.4182(4) -0.1685(4) 0.9041(3) 0.0178(11) Uani 1 1 d . . .
C27 C 0.4075(4) -0.0734(4) 0.9129(3) 0.0179(11) Uani 1 1 d . . .
H27A H 0.4122 -0.0750 0.9589 0.021 Uiso 1 1 calc R . .
C28 C 0.3671(5) 0.1130(4) 0.8729(3) 0.0201(12) Uani 1 1 d . . .
H28A H 0.2919 0.1487 0.8667 0.024 Uiso 1 1 calc R . .
C29 C 0.3964(5) 0.1064(5) 0.9439(3) 0.0251(13) Uani 1 1 d . . .
H29A H 0.4706 0.0703 0.9525 0.030 Uiso 1 1 calc R . .
H29B H 0.3620 0.0669 0.9805 0.030 Uiso 1 1 calc R . .
C30 C 0.3655(5) 0.2148(5) 0.9468(3) 0.0288(14) Uani 1 1 d . . .
H30A H 0.2906 0.2472 0.9439 0.035 Uiso 1 1 calc R . .
H30B H 0.3890 0.2099 0.9918 0.035 Uiso 1 1 calc R . .
C31 C 0.4097(5) 0.2821(5) 0.8882(3) 0.0300(14) Uani 1 1 d . . .
H31A H 0.4844 0.2547 0.8946 0.036 Uiso 1 1 calc R . .
H31B H 0.3837 0.3524 0.8901 0.036 Uiso 1 1 calc R . .
C32 C 0.3821(5) 0.2862(5) 0.8171(3) 0.0239(12) Uani 1 1 d . . .
H32A H 0.3079 0.3209 0.8082 0.029 Uiso 1 1 calc R . .
H32B H 0.4158 0.3264 0.7804 0.029 Uiso 1 1 calc R . .
C33 C 0.4149(4) 0.1791(4) 0.8146(3) 0.0190(11) Uani 1 1 d . . .
H33A H 0.4902 0.1469 0.8227 0.023 Uiso 1 1 calc R . .
C34 C 0.3634(5) 0.2509(5) 0.6915(3) 0.0261(13) Uani 1 1 d . . .
H34A H 0.3533 0.3162 0.6937 0.031 Uiso 1 1 calc R . .
C35 C 0.3470(5) 0.2460(5) 0.6254(3) 0.0240(13) Uani 1 1 d . . .
C36 C 0.3180(6) 0.3397(5) 0.5693(4) 0.0409(18) Uani 1 1 d . . .
H36A H 0.3038 0.4016 0.5781 0.049 Uiso 1 1 calc R . .
C37 C 0.3095(7) 0.3443(6) 0.5024(4) 0.053(2) Uani 1 1 d . . .
H37A H 0.2889 0.4088 0.4658 0.064 Uiso 1 1 calc R . .
C38 C 0.3307(6) 0.2559(6) 0.4884(3) 0.0352(16) Uani 1 1 d . . .
H38A H 0.3272 0.2588 0.4419 0.042 Uiso 1 1 calc R . .
C39 C 0.3573(5) 0.1622(5) 0.5420(3) 0.0257(13) Uani 1 1 d . . .
H39A H 0.3703 0.1016 0.5318 0.031 Uiso 1 1 calc R . .
C40 C 0.3655(4) 0.1548(5) 0.6108(3) 0.0204(12) Uani 1 1 d . . .
C41 C -0.2373(5) 0.3426(5) 0.7452(3) 0.0261(13) Uani 1 1 d . . .
C42 C -0.2346(5) 0.3345(5) 0.8140(4) 0.0318(15) Uani 1 1 d . . .
H42A H -0.1717 0.3097 0.8384 0.038 Uiso 1 1 calc R . .
C43 C -0.3271(7) 0.3639(6) 0.8470(4) 0.044(2) Uani 1 1 d . . .
H43A H -0.3268 0.3575 0.8945 0.053 Uiso 1 1 calc R . .
C44 C -0.4183(6) 0.4019(5) 0.8111(5) 0.049(2) Uani 1 1 d . . .
H44A H -0.4802 0.4235 0.8336 0.059 Uiso 1 1 calc R . .
C45 C -0.4199(5) 0.4086(5) 0.7435(4) 0.0394(18) Uani 1 1 d . . .
H45A H -0.4827 0.4326 0.7193 0.047 Uiso 1 1 calc R . .
C46 C -0.3286(5) 0.3800(5) 0.7100(4) 0.0332(16) Uani 1 1 d . . .
H46A H -0.3297 0.3865 0.6626 0.040 Uiso 1 1 calc R . .
C47 C -0.0790(4) 0.4155(4) 0.6704(3) 0.0210(12) Uani 1 1 d . . .
C48 C -0.1161(5) 0.4914(5) 0.7000(3) 0.0290(14) Uani 1 1 d . . .
H48A H -0.1629 0.4865 0.7363 0.035 Uiso 1 1 calc R . .
C49 C -0.0844(6) 0.5753(5) 0.6764(4) 0.0379(16) Uani 1 1 d . . .
H49A H -0.1114 0.6279 0.6962 0.046 Uiso 1 1 calc R . .
C50 C -0.0155(5) 0.5833(5) 0.6255(4) 0.0328(15) Uani 1 1 d . . .
H50A H 0.0077 0.6391 0.6113 0.039 Uiso 1 1 calc R . .
C51 C 0.0204(5) 0.5078(5) 0.5945(4) 0.0316(15) Uani 1 1 d . . .
H51A H 0.0661 0.5139 0.5576 0.038 Uiso 1 1 calc R . .
C52 C -0.0104(5) 0.4239(5) 0.6174(3) 0.0274(14) Uani 1 1 d . . .
H52A H 0.0155 0.3722 0.5968 0.033 Uiso 1 1 calc R . .
C53 C -0.1419(4) 0.2794(5) 0.6280(3) 0.0204(12) Uani 1 1 d . . .
C54 C -0.1645(5) 0.3527(5) 0.5620(3) 0.0285(14) Uani 1 1 d . . .
H54A H -0.1709 0.4213 0.5542 0.034 Uiso 1 1 calc R . .
C55 C -0.1778(5) 0.3240(6) 0.5074(3) 0.0366(17) Uani 1 1 d . . .
H55A H -0.1941 0.3738 0.4621 0.044 Uiso 1 1 calc R . .
C56 C -0.1675(6) 0.2247(7) 0.5180(4) 0.0382(17) Uani 1 1 d . . .
H56A H -0.1750 0.2056 0.4801 0.046 Uiso 1 1 calc R . .
C57 C -0.1465(6) 0.1533(6) 0.5838(4) 0.0381(16) Uani 1 1 d . . .
H57A H -0.1409 0.0850 0.5913 0.046 Uiso 1 1 calc R . .
C58 C -0.1333(5) 0.1797(5) 0.6394(3) 0.0273(13) Uani 1 1 d . . .
H58A H -0.1185 0.1298 0.6848 0.033 Uiso 1 1 calc R . .
C59 C 0.7455(5) -0.1472(5) 0.7570(3) 0.0282(14) Uani 1 1 d . . .
C60 C 0.7594(5) -0.1974(5) 0.8287(4) 0.0317(15) Uani 1 1 d . . .
H60A H 0.7022 -0.1908 0.8575 0.038 Uiso 1 1 calc R . .
C61 C 0.8550(6) -0.2564(6) 0.8581(4) 0.0413(18) Uani 1 1 d . . .
H61A H 0.8638 -0.2893 0.9070 0.050 Uiso 1 1 calc R . .
C62 C 0.9392(5) -0.2679(6) 0.8162(5) 0.044(2) Uani 1 1 d . . .
H62A H 1.0051 -0.3106 0.8362 0.053 Uiso 1 1 calc R . .
C63 C 0.9263(6) -0.2172(7) 0.7456(5) 0.045(2) Uani 1 1 d . . .
H63A H 0.9838 -0.2235 0.7173 0.054 Uiso 1 1 calc R . .
C64 C 0.8298(5) -0.1566(5) 0.7151(4) 0.0315(15) Uani 1 1 d . . .
H64A H 0.8215 -0.1220 0.6663 0.038 Uiso 1 1 calc R . .
C65 C 0.5894(5) -0.1813(4) 0.7015(3) 0.0205(12) Uani 1 1 d . . .
C66 C 0.6480(5) -0.2846(5) 0.7321(3) 0.0257(13) Uani 1 1 d . . .
H66A H 0.7073 -0.3036 0.7588 0.031 Uiso 1 1 calc R . .
C67 C 0.6210(5) -0.3603(5) 0.7242(4) 0.0337(15) Uani 1 1 d . . .
H67A H 0.6620 -0.4305 0.7451 0.040 Uiso 1 1 calc R . .
C68 C 0.5343(5) -0.3335(5) 0.6857(3) 0.0303(14) Uani 1 1 d . . .
H68A H 0.5160 -0.3853 0.6799 0.036 Uiso 1 1 calc R . .
C69 C 0.4743(5) -0.2308(5) 0.6558(3) 0.0300(14) Uani 1 1 d . . .
H69A H 0.4132 -0.2123 0.6311 0.036 Uiso 1 1 calc R . .
C70 C 0.5032(5) -0.1548(5) 0.6619(3) 0.0298(14) Uani 1 1 d . . .
H70A H 0.4640 -0.0845 0.6389 0.036 Uiso 1 1 calc R . .
C71 C 0.6226(4) 0.0133(5) 0.6368(3) 0.0213(12) Uani 1 1 d . . .
C72 C 0.6354(6) -0.0030(5) 0.5743(3) 0.0336(15) Uani 1 1 d . . .
H72A H 0.6441 -0.0684 0.5729 0.040 Uiso 1 1 calc R . .
C73 C 0.6354(7) 0.0765(6) 0.5135(4) 0.0413(18) Uani 1 1 d . . .
H73A H 0.6453 0.0652 0.4704 0.050 Uiso 1 1 calc R . .
C74 C 0.6210(6) 0.1721(5) 0.5156(4) 0.0369(16) Uani 1 1 d . . .
H74A H 0.6197 0.2267 0.4738 0.044 Uiso 1 1 calc R . .
C75 C 0.6085(6) 0.1885(6) 0.5782(4) 0.0371(17) Uani 1 1 d . . .
H75A H 0.5993 0.2540 0.5797 0.045 Uiso 1 1 calc R . .
C76 C 0.6097(5) 0.1087(5) 0.6386(3) 0.0290(14) Uani 1 1 d . . .
H76A H 0.6014 0.1195 0.6819 0.035 Uiso 1 1 calc R . .
C77 C 0.7067(8) 0.5497(10) 0.9290(6) 0.072(3) Uani 1 1 d . . .
H77A H 0.6688 0.6216 0.9001 0.086 Uiso 1 1 calc R . .
H77B H 0.6637 0.5091 0.9329 0.086 Uiso 1 1 calc R . .
Cl1 Cl 0.7293(3) 0.5459(3) 1.0102(2) 0.0988(11) Uani 1 1 d . . .
Cl2 Cl 0.81881(17) 0.50124(19) 0.88777(13) 0.0567(5) Uani 1 1 d . . .
C78 C 0.528(5) 0.450(3) 0.5035(17) 0.23(3) Uiso 0.50 1 d PD . .
Cl3 Cl 0.4729(5) 0.5210(5) 0.5557(3) 0.0753(14) Uiso 0.50 1 d PD . .
Cl4 Cl 0.4890(7) 0.4555(7) 0.5931(4) 0.109(2) Uiso 0.50 1 d PD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os1 0.01399(13) 0.01724(13) 0.01007(12) -0.00358(9) 0.00140(8) -0.00712(9)
Os2 0.01425(13) 0.01580(13) 0.01156(12) -0.00383(9) 0.00142(8) -0.00708(9)
P1 0.0154(7) 0.0179(7) 0.0157(6) -0.0050(5) 0.0035(5) -0.0056(5)
P2 0.0158(7) 0.0193(7) 0.0190(7) -0.0092(5) 0.0018(5) -0.0052(5)
P3 0.0255(8) 0.0301(8) 0.0267(8) -0.0086(6) 0.0042(6) -0.0105(7)
P4 0.0231(7) 0.0218(7) 0.0166(7) -0.0060(6) 0.0019(5) -0.0100(6)
F1 0.107(5) 0.055(3) 0.093(4) -0.034(3) 0.022(4) -0.053(4)
F2 0.049(3) 0.093(4) 0.043(3) -0.005(3) 0.023(2) -0.027(3)
F3 0.038(3) 0.082(4) 0.045(3) -0.012(2) -0.011(2) -0.012(3)
F4 0.082(4) 0.049(3) 0.063(3) -0.034(3) -0.006(3) -0.012(3)
F5 0.035(3) 0.065(3) 0.058(3) -0.003(3) -0.012(2) 0.005(2)
F6 0.053(3) 0.075(3) 0.041(2) -0.024(2) 0.022(2) -0.041(3)
F7 0.035(2) 0.038(2) 0.038(2) -0.0165(17) -0.0001(16) -0.0208(18)
F8 0.070(4) 0.076(4) 0.062(3) -0.054(3) 0.036(3) -0.043(3)
F9 0.055(3) 0.035(2) 0.065(3) 0.014(2) -0.028(2) -0.022(2)
F10 0.058(3) 0.076(4) 0.059(3) -0.052(3) 0.036(2) -0.042(3)
F11 0.059(3) 0.038(3) 0.065(3) 0.016(2) -0.028(3) -0.016(2)
F12 0.032(2) 0.036(2) 0.038(2) -0.0146(17) 0.0080(16) -0.0209(17)
O1 0.025(2) 0.024(2) 0.0080(17) 0.0031(15) -0.0035(15) -0.0041(17)
O2 0.0192(19) 0.022(2) 0.0142(18) -0.0034(15) -0.0015(14) -0.0130(16)
O3 0.024(2) 0.020(2) 0.0149(18) -0.0030(15) -0.0021(15) -0.0162(17)
O4 0.026(2) 0.025(2) 0.0079(17) -0.0076(15) 0.0038(14) -0.0083(17)
O5 0.033(2) 0.021(2) 0.0037(17) -0.0003(14) 0.0045(15) -0.0171(18)
N1 0.012(2) 0.018(2) 0.015(2) -0.0040(18) 0.0004(16) -0.0090(18)
N2 0.022(2) 0.021(2) 0.012(2) 0.0038(18) -0.0015(17) -0.009(2)
N3 0.019(2) 0.017(2) 0.011(2) -0.0112(17) 0.0013(16) -0.0069(18)
N4 0.011(2) 0.016(2) 0.021(2) -0.0065(18) 0.0031(17) -0.0109(17)
N5 0.030(3) 0.020(2) 0.010(2) 0.0013(18) 0.0013(18) -0.014(2)
N6 0.020(2) 0.025(3) 0.014(2) -0.0088(19) 0.0022(18) -0.008(2)
C1 0.017(3) 0.026(3) 0.015(3) -0.014(2) -0.001(2) -0.004(2)
C2 0.022(3) 0.028(3) 0.021(3) -0.007(2) 0.003(2) -0.003(2)
C3 0.058(5) 0.044(4) 0.014(3) -0.012(3) 0.001(3) -0.010(4)
C4 0.082(6) 0.035(4) 0.022(3) -0.017(3) 0.000(3) -0.011(4)
C5 0.060(5) 0.022(3) 0.027(3) -0.017(3) 0.002(3) -0.006(3)
C6 0.027(3) 0.026(3) 0.020(3) -0.011(2) 0.000(2) -0.001(3)
C7 0.023(3) 0.021(3) 0.023(3) -0.013(2) 0.003(2) -0.007(2)
C8 0.026(3) 0.022(3) 0.017(3) -0.003(2) 0.004(2) -0.018(2)
C9 0.034(3) 0.025(3) 0.019(3) -0.006(2) 0.000(2) -0.013(3)
C10 0.047(4) 0.028(3) 0.023(3) -0.005(3) 0.005(3) -0.016(3)
C11 0.036(4) 0.029(3) 0.019(3) 0.004(2) -0.007(2) -0.020(3)
C12 0.033(3) 0.028(3) 0.015(3) -0.005(2) 0.006(2) -0.015(3)
C13 0.024(3) 0.021(3) 0.017(3) -0.005(2) 0.003(2) -0.014(2)
C14 0.020(3) 0.026(3) 0.011(2) -0.008(2) 0.004(2) -0.012(2)
C15 0.017(3) 0.027(3) 0.022(3) -0.016(2) 0.003(2) -0.008(2)
C16 0.026(3) 0.025(3) 0.020(3) -0.010(2) 0.002(2) -0.007(2)
C17 0.031(4) 0.033(4) 0.033(3) -0.020(3) 0.000(3) -0.006(3)
C18 0.035(4) 0.020(3) 0.038(4) -0.016(3) 0.000(3) -0.008(3)
C19 0.028(3) 0.019(3) 0.023(3) -0.007(2) 0.001(2) -0.010(2)
C20 0.012(3) 0.023(3) 0.023(3) -0.008(2) 0.001(2) -0.006(2)
C21 0.018(3) 0.022(3) 0.019(3) -0.001(2) 0.001(2) -0.003(2)
C22 0.026(3) 0.024(3) 0.020(3) -0.011(2) 0.002(2) -0.010(2)
C23 0.027(3) 0.018(3) 0.023(3) -0.006(2) 0.005(2) -0.010(2)
C24 0.034(3) 0.021(3) 0.021(3) -0.003(2) 0.002(2) -0.012(3)
C25 0.027(3) 0.023(3) 0.019(3) -0.005(2) 0.000(2) -0.011(2)
C26 0.015(3) 0.022(3) 0.018(3) -0.008(2) 0.002(2) -0.007(2)
C27 0.019(3) 0.022(3) 0.009(2) -0.005(2) 0.0026(19) -0.005(2)
C28 0.022(3) 0.020(3) 0.021(3) -0.007(2) 0.001(2) -0.010(2)
C29 0.036(4) 0.025(3) 0.017(3) -0.008(2) -0.002(2) -0.012(3)
C30 0.036(4) 0.030(3) 0.027(3) -0.016(3) 0.007(3) -0.015(3)
C31 0.036(4) 0.028(3) 0.033(3) -0.017(3) 0.001(3) -0.013(3)
C32 0.030(3) 0.024(3) 0.023(3) -0.010(2) 0.000(2) -0.012(3)
C33 0.020(3) 0.022(3) 0.021(3) -0.010(2) -0.001(2) -0.012(2)
C34 0.029(3) 0.020(3) 0.024(3) -0.007(2) 0.004(2) -0.005(2)
C35 0.025(3) 0.023(3) 0.019(3) -0.004(2) 0.002(2) -0.006(2)
C36 0.063(5) 0.020(3) 0.029(4) -0.004(3) 0.003(3) -0.007(3)
C37 0.086(7) 0.023(4) 0.023(4) 0.007(3) -0.005(4) -0.002(4)
C38 0.047(4) 0.037(4) 0.013(3) 0.000(3) -0.002(3) -0.012(3)
C39 0.026(3) 0.025(3) 0.024(3) -0.006(2) 0.003(2) -0.009(3)
C40 0.018(3) 0.021(3) 0.012(3) 0.002(2) 0.007(2) -0.004(2)
C41 0.023(3) 0.020(3) 0.033(3) -0.009(2) 0.012(2) -0.008(2)
C42 0.037(4) 0.019(3) 0.033(3) -0.009(3) 0.019(3) -0.007(3)
C43 0.057(5) 0.028(4) 0.047(4) -0.017(3) 0.036(4) -0.020(3)
C44 0.032(4) 0.021(3) 0.090(7) -0.021(4) 0.039(4) -0.012(3)
C45 0.020(3) 0.027(3) 0.067(5) -0.015(3) 0.018(3) -0.010(3)
C46 0.023(3) 0.021(3) 0.048(4) -0.008(3) 0.010(3) -0.005(3)
C47 0.018(3) 0.021(3) 0.022(3) -0.004(2) 0.002(2) -0.010(2)
C48 0.033(4) 0.023(3) 0.027(3) -0.007(2) 0.009(3) -0.011(3)
C49 0.046(4) 0.025(3) 0.047(4) -0.018(3) 0.010(3) -0.016(3)
C50 0.036(4) 0.025(3) 0.036(4) -0.003(3) -0.002(3) -0.016(3)
C51 0.034(4) 0.025(3) 0.036(4) -0.007(3) 0.016(3) -0.018(3)
C52 0.036(4) 0.021(3) 0.023(3) -0.005(2) 0.010(3) -0.013(3)
C53 0.016(3) 0.027(3) 0.017(3) -0.010(2) 0.000(2) -0.003(2)
C54 0.024(3) 0.025(3) 0.028(3) -0.005(3) -0.003(2) -0.003(3)
C55 0.032(4) 0.053(5) 0.021(3) -0.006(3) -0.004(3) -0.017(3)
C56 0.046(4) 0.060(5) 0.027(3) -0.026(3) 0.004(3) -0.028(4)
C57 0.048(4) 0.042(4) 0.036(4) -0.019(3) -0.003(3) -0.023(3)
C58 0.029(3) 0.029(3) 0.023(3) -0.008(2) -0.004(2) -0.010(3)
C59 0.032(4) 0.023(3) 0.036(3) -0.019(3) 0.001(3) -0.009(3)
C60 0.030(4) 0.028(3) 0.035(4) -0.012(3) -0.010(3) -0.004(3)
C61 0.044(4) 0.028(4) 0.049(4) -0.013(3) -0.023(3) -0.003(3)
C62 0.021(3) 0.031(4) 0.082(6) -0.025(4) -0.019(4) -0.002(3)
C63 0.021(3) 0.052(5) 0.082(6) -0.048(5) 0.010(4) -0.012(3)
C64 0.021(3) 0.035(4) 0.046(4) -0.024(3) 0.006(3) -0.009(3)
C65 0.028(3) 0.020(3) 0.021(3) -0.013(2) 0.006(2) -0.012(2)
C66 0.020(3) 0.023(3) 0.031(3) -0.006(2) -0.003(2) -0.005(2)
C67 0.026(3) 0.019(3) 0.054(4) -0.010(3) -0.007(3) -0.006(3)
C68 0.037(4) 0.024(3) 0.033(3) -0.013(3) 0.003(3) -0.011(3)
C69 0.040(4) 0.025(3) 0.027(3) -0.008(3) -0.009(3) -0.012(3)
C70 0.039(4) 0.022(3) 0.028(3) -0.008(2) -0.007(3) -0.008(3)
C71 0.016(3) 0.026(3) 0.020(3) -0.008(2) 0.009(2) -0.007(2)
C72 0.052(4) 0.027(3) 0.024(3) -0.010(3) 0.003(3) -0.016(3)
C73 0.067(5) 0.035(4) 0.023(3) -0.008(3) 0.005(3) -0.023(4)
C74 0.048(4) 0.031(4) 0.030(3) 0.000(3) 0.004(3) -0.023(3)
C75 0.047(4) 0.030(4) 0.043(4) -0.015(3) 0.017(3) -0.025(3)
C76 0.036(4) 0.031(3) 0.028(3) -0.014(3) 0.009(3) -0.019(3)
C77 0.042(5) 0.094(9) 0.094(8) -0.053(7) 0.015(5) -0.025(5)
Cl1 0.087(2) 0.125(3) 0.103(2) -0.084(2) 0.0222(18) -0.022(2)
Cl2 0.0443(11) 0.0611(13) 0.0673(13) -0.0319(11) 0.0076(10) -0.0139(10)

_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 O5 1.820(4) . ?
Os1 N1 2.001(5) . ?
Os1 O2 2.019(4) . ?
Os1 N2 2.026(4) . ?
Os1 N5 2.034(5) . ?
Os1 O1 2.034(4) . ?
Os2 O5 1.828(4) . ?
Os2 N3 2.009(4) . ?
Os2 N4 2.012(4) . ?
Os2 O3 2.023(4) . ?
Os2 O4 2.036(4) . ?
Os2 N6 2.047(5) . ?
P1 N5 1.614(5) . ?
P1 C47 1.801(6) . ?
P1 C53 1.804(6) . ?
P1 C41 1.809(6) . ?
P2 N6 1.627(5) . ?
P2 C71 1.798(6) . ?
P2 C59 1.800(7) . ?
P2 C65 1.800(6) . ?
P3 F5 1.573(5) . ?
P3 F1 1.584(6) . ?
P3 F2 1.586(4) . ?
P3 F4 1.588(5) . ?
P3 F6 1.593(4) . ?
P3 F3 1.613(5) . ?
P4 F11 1.579(4) . ?
P4 F9 1.584(4) . ?
P4 F8 1.587(4) . ?
P4 F10 1.590(4) . ?
P4 F7 1.611(4) . ?
P4 F12 1.626(4) . ?
O1 C1 1.323(7) . ?
O2 C20 1.329(7) . ?
O3 C21 1.324(7) . ?
O4 C40 1.330(7) . ?
N1 C7 1.296(8) . ?
N1 C8 1.489(7) . ?
N2 C14 1.301(8) . ?
N2 C13 1.454(7) . ?
N3 C27 1.312(7) . ?
N3 C28 1.465(7) . ?
N4 C34 1.314(8) . ?
N4 C33 1.476(7) . ?
N5 H5N 0.8800 . ?
N6 H6N 0.8800 . ?
C1 C2 1.409(8) . ?
C1 C6 1.413(9) . ?
C2 C3 1.365(10) . ?
C2 H2A 0.9500 . ?
C3 C4 1.393(11) . ?
C3 H3A 0.9500 . ?
C4 C5 1.376(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.431(9) . ?
C5 H5A 0.9500 . ?
C6 C7 1.434(8) . ?
C7 H7A 0.9500 . ?
C8 C9 1.495(8) . ?
C8 C13 1.554(8) . ?
C8 H8A 1.0000 . ?
C9 C10 1.516(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.521(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.528(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.528(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 1.0000 . ?
C14 C15 1.440(8) . ?
C14 H14A 0.9500 . ?
C15 C16 1.423(8) . ?
C15 C20 1.424(8) . ?
C16 C17 1.368(9) . ?
C16 H16A 0.9500 . ?
C17 C18 1.406(10) . ?
C17 H17A 0.9500 . ?
C18 C19 1.345(9) . ?
C18 H18A 0.9500 . ?
C19 C20 1.417(8) . ?
C19 H19A 0.9500 . ?
C21 C22 1.399(9) . ?
C21 C26 1.432(8) . ?
C22 C23 1.370(8) . ?
C22 H22A 0.9500 . ?
C23 C24 1.412(9) . ?
C23 H23A 0.9500 . ?
C24 C25 1.358(9) . ?
C24 H24A 0.9500 . ?
C25 C26 1.421(8) . ?
C25 H25A 0.9500 . ?
C26 C27 1.447(8) . ?
C27 H27A 0.9500 . ?
C28 C29 1.524(8) . ?
C28 C33 1.540(8) . ?
C28 H28A 1.0000 . ?
C29 C30 1.534(9) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.522(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.532(8) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.510(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 1.0000 . ?
C34 C35 1.438(9) . ?
C34 H34A 0.9500 . ?
C35 C36 1.409(9) . ?
C35 C40 1.425(9) . ?
C36 C37 1.373(11) . ?
C36 H36A 0.9500 . ?
C37 C38 1.371(11) . ?
C37 H37A 0.9500 . ?
C38 C39 1.385(9) . ?
C38 H38A 0.9500 . ?
C39 C40 1.396(9) . ?
C39 H39A 0.9500 . ?
C41 C46 1.375(10) . ?
C41 C42 1.384(10) . ?
C42 C43 1.408(9) . ?
C42 H42A 0.9500 . ?
C43 C44 1.379(13) . ?
C43 H43A 0.9500 . ?
C44 C45 1.364(13) . ?
C44 H44A 0.9500 . ?
C45 C46 1.398(9) . ?
C45 H45A 0.9500 . ?
C46 H46A 0.9500 . ?
C47 C48 1.385(9) . ?
C47 C52 1.392(8) . ?
C48 C49 1.399(9) . ?
C48 H48A 0.9500 . ?
C49 C50 1.364(10) . ?
C49 H49A 0.9500 . ?
C50 C51 1.400(10) . ?
C50 H50A 0.9500 . ?
C51 C52 1.390(9) . ?
C51 H51A 0.9500 . ?
C52 H52A 0.9500 . ?
C53 C58 1.383(9) . ?
C53 C54 1.388(9) . ?
C54 C55 1.391(10) . ?
C54 H54A 0.9500 . ?
C55 C56 1.374(11) . ?
C55 H55A 0.9500 . ?
C56 C57 1.373(11) . ?
C56 H56A 0.9500 . ?
C57 C58 1.390(10) . ?
C57 H57A 0.9500 . ?
C58 H58A 0.9500 . ?
C59 C64 1.396(9) . ?
C59 C60 1.397(10) . ?
C60 C61 1.375(10) . ?
C60 H60A 0.9500 . ?
C61 C62 1.395(12) . ?
C61 H61A 0.9500 . ?
C62 C63 1.377(13) . ?
C62 H62A 0.9500 . ?
C63 C64 1.395(11) . ?
C63 H63A 0.9500 . ?
C64 H64A 0.9500 . ?
C65 C66 1.390(8) . ?
C65 C70 1.394(9) . ?
C66 C67 1.386(9) . ?
C66 H66A 0.9500 . ?
C67 C68 1.385(10) . ?
C67 H67A 0.9500 . ?
C68 C69 1.388(9) . ?
C68 H68A 0.9500 . ?
C69 C70 1.392(9) . ?
C69 H69A 0.9500 . ?
C70 H70A 0.9500 . ?
C71 C72 1.376(9) . ?
C71 C76 1.382(9) . ?
C72 C73 1.387(10) . ?
C72 H72A 0.9500 . ?
C73 C74 1.383(11) . ?
C73 H73A 0.9500 . ?
C74 C75 1.379(10) . ?
C74 H74A 0.9500 . ?
C75 C76 1.382(10) . ?
C75 H75A 0.9500 . ?
C76 H76A 0.9500 . ?
C77 Cl1 1.714(12) . ?
C77 Cl2 1.757(10) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
C78 Cl3 1.14(3) 2_666 ?
C78 C78 1.38(8) 2_666 ?
C78 Cl3 1.712(18) . ?
C78 Cl4 1.898(19) . ?
C78 Cl4 1.97(4) 2_666 ?
Cl3 Cl4 0.969(10) . ?
Cl3 C78 1.14(3) 2_666 ?
Cl4 C78 1.97(4) 2_666 ?

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
O5 Os1 N1 91.46(17) . . ?
O5 Os1 O2 90.11(16) . . ?
N1 Os1 O2 176.61(16) . . ?
O5 Os1 N2 91.11(17) . . ?
N1 Os1 N2 82.49(19) . . ?
O2 Os1 N2 94.48(18) . . ?
O5 Os1 N5 176.34(19) . . ?
N1 Os1 N5 91.65(19) . . ?
O2 Os1 N5 86.68(18) . . ?
N2 Os1 N5 87.39(19) . . ?
O5 Os1 O1 92.33(16) . . ?
N1 Os1 O1 93.38(18) . . ?
O2 Os1 O1 89.55(17) . . ?
N2 Os1 O1 174.69(19) . . ?
N5 Os1 O1 89.40(17) . . ?
O5 Os2 N3 91.30(17) . . ?
O5 Os2 N4 90.42(17) . . ?
N3 Os2 N4 82.66(18) . . ?
O5 Os2 O3 89.77(16) . . ?
N3 Os2 O3 94.43(17) . . ?
N4 Os2 O3 177.09(16) . . ?
O5 Os2 O4 90.99(16) . . ?
N3 Os2 O4 174.78(17) . . ?
N4 Os2 O4 92.63(18) . . ?
O3 Os2 O4 90.27(16) . . ?
O5 Os2 N6 176.43(17) . . ?
N3 Os2 N6 86.67(18) . . ?
N4 Os2 N6 92.23(19) . . ?
O3 Os2 N6 87.46(18) . . ?
O4 Os2 N6 91.27(17) . . ?
N5 P1 C47 114.7(3) . . ?
N5 P1 C53 111.3(3) . . ?
C47 P1 C53 107.9(3) . . ?
N5 P1 C41 106.3(3) . . ?
C47 P1 C41 108.1(3) . . ?
C53 P1 C41 108.3(3) . . ?
N6 P2 C71 110.5(3) . . ?
N6 P2 C59 108.6(3) . . ?
C71 P2 C59 108.3(3) . . ?
N6 P2 C65 113.9(3) . . ?
C71 P2 C65 109.2(3) . . ?
C59 P2 C65 106.1(3) . . ?
F5 P3 F1 91.3(4) . . ?
F5 P3 F2 90.9(3) . . ?
F1 P3 F2 91.2(3) . . ?
F5 P3 F4 90.0(3) . . ?
F1 P3 F4 178.4(4) . . ?
F2 P3 F4 89.7(3) . . ?
F5 P3 F6 90.3(3) . . ?
F1 P3 F6 89.6(3) . . ?
F2 P3 F6 178.5(3) . . ?
F4 P3 F6 89.4(3) . . ?
F5 P3 F3 179.2(3) . . ?
F1 P3 F3 89.4(4) . . ?
F2 P3 F3 89.6(3) . . ?
F4 P3 F3 89.3(3) . . ?
F6 P3 F3 89.2(3) . . ?
F11 P4 F9 179.4(4) . . ?
F11 P4 F8 89.8(3) . . ?
F9 P4 F8 90.8(3) . . ?
F11 P4 F10 90.0(3) . . ?
F9 P4 F10 89.4(3) . . ?
F8 P4 F10 179.5(3) . . ?
F11 P4 F7 90.4(3) . . ?
F9 P4 F7 89.8(2) . . ?
F8 P4 F7 90.8(2) . . ?
F10 P4 F7 89.6(2) . . ?
F11 P4 F12 90.5(3) . . ?
F9 P4 F12 89.4(2) . . ?
F8 P4 F12 89.7(2) . . ?
F10 P4 F12 89.9(2) . . ?
F7 P4 F12 179.0(2) . . ?
C1 O1 Os1 123.3(4) . . ?
C20 O2 Os1 122.8(3) . . ?
C21 O3 Os2 123.6(4) . . ?
C40 O4 Os2 122.5(4) . . ?
Os1 O5 Os2 178.1(2) . . ?
C7 N1 C8 120.2(5) . . ?
C7 N1 Os1 125.0(4) . . ?
C8 N1 Os1 114.8(4) . . ?
C14 N2 C13 125.3(5) . . ?
C14 N2 Os1 123.6(4) . . ?
C13 N2 Os1 110.7(4) . . ?
C27 N3 C28 124.6(5) . . ?
C27 N3 Os2 123.6(4) . . ?
C28 N3 Os2 111.6(3) . . ?
C34 N4 C33 122.6(5) . . ?
C34 N4 Os2 124.1(4) . . ?
C33 N4 Os2 112.9(3) . . ?
P1 N5 Os1 129.6(3) . . ?
P1 N5 H5N 115.2 . . ?
Os1 N5 H5N 115.2 . . ?
P2 N6 Os2 127.6(3) . . ?
P2 N6 H6N 116.2 . . ?
Os2 N6 H6N 116.2 . . ?
O1 C1 C2 115.9(5) . . ?
O1 C1 C6 125.0(5) . . ?
C2 C1 C6 119.1(5) . . ?
C3 C2 C1 121.2(6) . . ?
C3 C2 H2A 119.4 . . ?
C1 C2 H2A 119.4 . . ?
C2 C3 C4 120.8(6) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 H3A 119.6 . . ?
C5 C4 C3 119.7(7) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 121.0(7) . . ?
C4 C5 H5A 119.5 . . ?
C6 C5 H5A 119.5 . . ?
C1 C6 C5 118.1(6) . . ?
C1 C6 C7 127.3(6) . . ?
C5 C6 C7 114.5(6) . . ?
N1 C7 C6 124.6(6) . . ?
N1 C7 H7A 117.7 . . ?
C6 C7 H7A 117.7 . . ?
N1 C8 C9 117.3(5) . . ?
N1 C8 C13 105.1(4) . . ?
C9 C8 C13 110.6(5) . . ?
N1 C8 H8A 107.8 . . ?
C9 C8 H8A 107.8 . . ?
C13 C8 H8A 107.8 . . ?
C8 C9 C10 111.0(5) . . ?
C8 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C9 C10 C11 111.2(6) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C10 C11 C12 113.0(5) . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 C13 110.7(5) . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N2 C13 C12 116.3(5) . . ?
N2 C13 C8 109.8(5) . . ?
C12 C13 C8 109.1(5) . . ?
N2 C13 H13A 107.1 . . ?
C12 C13 H13A 107.1 . . ?
C8 C13 H13A 107.1 . . ?
N2 C14 C15 125.5(5) . . ?
N2 C14 H14A 117.2 . . ?
C15 C14 H14A 117.2 . . ?
C16 C15 C20 118.7(6) . . ?
C16 C15 C14 114.5(5) . . ?
C20 C15 C14 126.7(5) . . ?
C17 C16 C15 121.6(6) . . ?
C17 C16 H16A 119.2 . . ?
C15 C16 H16A 119.2 . . ?
C16 C17 C18 118.7(6) . . ?
C16 C17 H17A 120.6 . . ?
C18 C17 H17A 120.6 . . ?
C19 C18 C17 121.6(6) . . ?
C19 C18 H18A 119.2 . . ?
C17 C18 H18A 119.2 . . ?
C18 C19 C20 121.6(6) . . ?
C18 C19 H19A 119.2 . . ?
C20 C19 H19A 119.2 . . ?
O2 C20 C19 116.6(5) . . ?
O2 C20 C15 125.5(5) . . ?
C19 C20 C15 117.9(5) . . ?
O3 C21 C22 116.6(6) . . ?
O3 C21 C26 124.6(6) . . ?
C22 C21 C26 118.7(5) . . ?
C23 C22 C21 122.0(6) . . ?
C23 C22 H22A 119.0 . . ?
C21 C22 H22A 119.0 . . ?
C22 C23 C24 120.0(6) . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
C25 C24 C23 119.2(5) . . ?
C25 C24 H24A 120.4 . . ?
C23 C24 H24A 120.4 . . ?
C24 C25 C26 122.6(6) . . ?
C24 C25 H25A 118.7 . . ?
C26 C25 H25A 118.7 . . ?
C25 C26 C21 117.5(6) . . ?
C25 C26 C27 115.7(5) . . ?
C21 C26 C27 126.6(5) . . ?
N3 C27 C26 125.5(5) . . ?
N3 C27 H27A 117.2 . . ?
C26 C27 H27A 117.2 . . ?
N3 C28 C29 115.9(5) . . ?
N3 C28 C33 108.2(5) . . ?
C29 C28 C33 111.0(5) . . ?
N3 C28 H28A 107.1 . . ?
C29 C28 H28A 107.1 . . ?
C33 C28 H28A 107.1 . . ?
C28 C29 C30 109.7(5) . . ?
C28 C29 H29A 109.7 . . ?
C30 C29 H29A 109.7 . . ?
C28 C29 H29B 109.7 . . ?
C30 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
C31 C30 C29 112.2(5) . . ?
C31 C30 H30A 109.2 . . ?
C29 C30 H30A 109.2 . . ?
C31 C30 H30B 109.2 . . ?
C29 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 C32 111.6(5) . . ?
C30 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
C30 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 108.0 . . ?
C33 C32 C31 110.3(5) . . ?
C33 C32 H32A 109.6 . . ?
C31 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
N4 C33 C32 116.2(5) . . ?
N4 C33 C28 106.6(4) . . ?
C32 C33 C28 111.0(5) . . ?
N4 C33 H33A 107.5 . . ?
C32 C33 H33A 107.5 . . ?
C28 C33 H33A 107.5 . . ?
N4 C34 C35 124.7(6) . . ?
N4 C34 H34A 117.7 . . ?
C35 C34 H34A 117.7 . . ?
C36 C35 C40 117.6(6) . . ?
C36 C35 C34 116.4(6) . . ?
C40 C35 C34 125.8(5) . . ?
C37 C36 C35 122.2(7) . . ?
C37 C36 H36A 118.9 . . ?
C35 C36 H36A 118.9 . . ?
C38 C37 C36 119.9(6) . . ?
C38 C37 H37A 120.1 . . ?
C36 C37 H37A 120.1 . . ?
C37 C38 C39 120.1(6) . . ?
C37 C38 H38A 120.0 . . ?
C39 C38 H38A 120.0 . . ?
C38 C39 C40 121.5(6) . . ?
C38 C39 H39A 119.3 . . ?
C40 C39 H39A 119.3 . . ?
O4 C40 C39 115.6(6) . . ?
O4 C40 C35 125.7(5) . . ?
C39 C40 C35 118.8(5) . . ?
C46 C41 C42 120.4(6) . . ?
C46 C41 P1 120.8(5) . . ?
C42 C41 P1 118.8(5) . . ?
C41 C42 C43 118.4(7) . . ?
C41 C42 H42A 120.8 . . ?
C43 C42 H42A 120.8 . . ?
C44 C43 C42 120.7(8) . . ?
C44 C43 H43A 119.6 . . ?
C42 C43 H43A 119.6 . . ?
C45 C44 C43 120.2(6) . . ?
C45 C44 H44A 119.9 . . ?
C43 C44 H44A 119.9 . . ?
C44 C45 C46 119.7(8) . . ?
C44 C45 H45A 120.2 . . ?
C46 C45 H45A 120.2 . . ?
C41 C46 C45 120.5(7) . . ?
C41 C46 H46A 119.7 . . ?
C45 C46 H46A 119.7 . . ?
C48 C47 C52 119.3(6) . . ?
C48 C47 P1 119.6(5) . . ?
C52 C47 P1 121.1(5) . . ?
C47 C48 C49 119.9(6) . . ?
C47 C48 H48A 120.1 . . ?
C49 C48 H48A 120.1 . . ?
C50 C49 C48 121.4(7) . . ?
C50 C49 H49A 119.3 . . ?
C48 C49 H49A 119.3 . . ?
C49 C50 C51 118.8(6) . . ?
C49 C50 H50A 120.6 . . ?
C51 C50 H50A 120.6 . . ?
C52 C51 C50 120.4(6) . . ?
C52 C51 H51A 119.8 . . ?
C50 C51 H51A 119.8 . . ?
C51 C52 C47 120.2(6) . . ?
C51 C52 H52A 119.9 . . ?
C47 C52 H52A 119.9 . . ?
C58 C53 C54 120.6(6) . . ?
C58 C53 P1 116.7(4) . . ?
C54 C53 P1 122.7(5) . . ?
C53 C54 C55 118.8(7) . . ?
C53 C54 H54A 120.6 . . ?
C55 C54 H54A 120.6 . . ?
C56 C55 C54 121.0(6) . . ?
C56 C55 H55A 119.5 . . ?
C54 C55 H55A 119.5 . . ?
C57 C56 C55 119.6(6) . . ?
C57 C56 H56A 120.2 . . ?
C55 C56 H56A 120.2 . . ?
C56 C57 C58 120.8(7) . . ?
C56 C57 H57A 119.6 . . ?
C58 C57 H57A 119.6 . . ?
C53 C58 C57 119.1(6) . . ?
C53 C58 H58A 120.4 . . ?
C57 C58 H58A 120.4 . . ?
C64 C59 C60 119.5(7) . . ?
C64 C59 P2 119.9(5) . . ?
C60 C59 P2 120.1(5) . . ?
C61 C60 C59 120.5(7) . . ?
C61 C60 H60A 119.7 . . ?
C59 C60 H60A 119.7 . . ?
C60 C61 C62 120.1(7) . . ?
C60 C61 H61A 119.9 . . ?
C62 C61 H61A 119.9 . . ?
C63 C62 C61 119.6(7) . . ?
C63 C62 H62A 120.2 . . ?
C61 C62 H62A 120.2 . . ?
C62 C63 C64 120.9(7) . . ?
C62 C63 H63A 119.5 . . ?
C64 C63 H63A 119.5 . . ?
C63 C64 C59 119.3(7) . . ?
C63 C64 H64A 120.4 . . ?
C59 C64 H64A 120.4 . . ?
C66 C65 C70 118.8(6) . . ?
C66 C65 P2 120.4(5) . . ?
C70 C65 P2 120.7(5) . . ?
C67 C66 C65 120.9(6) . . ?
C67 C66 H66A 119.5 . . ?
C65 C66 H66A 119.5 . . ?
C68 C67 C66 120.1(6) . . ?
C68 C67 H67A 120.0 . . ?
C66 C67 H67A 120.0 . . ?
C67 C68 C69 119.6(6) . . ?
C67 C68 H68A 120.2 . . ?
C69 C68 H68A 120.2 . . ?
C68 C69 C70 120.3(6) . . ?
C68 C69 H69A 119.9 . . ?
C70 C69 H69A 119.9 . . ?
C69 C70 C65 120.2(6) . . ?
C69 C70 H70A 119.9 . . ?
C65 C70 H70A 119.9 . . ?
C72 C71 C76 119.9(6) . . ?
C72 C71 P2 122.8(5) . . ?
C76 C71 P2 117.2(5) . . ?
C71 C72 C73 119.7(7) . . ?
C71 C72 H72A 120.1 . . ?
C73 C72 H72A 120.1 . . ?
C74 C73 C72 120.1(7) . . ?
C74 C73 H73A 120.0 . . ?
C72 C73 H73A 120.0 . . ?
C75 C74 C73 120.3(6) . . ?
C75 C74 H74A 119.9 . . ?
C73 C74 H74A 119.9 . . ?
C74 C75 C76 119.4(7) . . ?
C74 C75 H75A 120.3 . . ?
C76 C75 H75A 120.3 . . ?
C71 C76 C75 120.6(6) . . ?
C71 C76 H76A 119.7 . . ?
C75 C76 H76A 119.7 . . ?
Cl1 C77 Cl2 112.6(6) . . ?
Cl1 C77 H77A 109.1 . . ?
Cl2 C77 H77A 109.1 . . ?
Cl1 C77 H77B 109.1 . . ?
Cl2 C77 H77B 109.1 . . ?
H77A C77 H77B 107.8 . . ?
Cl3 C78 C78 85(4) 2_666 2_666 ?
Cl3 C78 Cl3 127(3) 2_666 . ?
C78 C78 Cl3 41.6(12) 2_666 . ?
Cl3 C78 Cl4 156(4) 2_666 . ?
C78 C78 Cl4 71.9(15) 2_666 . ?
Cl3 C78 Cl4 30.6(4) . . ?
Cl3 C78 Cl4 19.4(13) 2_666 2_666 ?
C78 C78 Cl4 66(3) 2_666 2_666 ?
Cl3 C78 Cl4 108(2) . 2_666 ?
Cl4 C78 Cl4 138(2) . 2_666 ?
Cl4 Cl3 C78 138(2) . 2_666 ?
Cl4 Cl3 C78 85.3(14) . . ?
C78 Cl3 C78 53(3) 2_666 . ?
Cl3 Cl4 C78 64.1(13) . . ?
Cl3 Cl4 C78 23.0(12) . 2_666 ?
C78 Cl4 C78 42(2) . 2_666 ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        66.99
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         2.302
_refine_diff_density_min         -2.241
_refine_diff_density_rms         0.177

data_4
_database_code_depnum_ccdc_archive 'CCDC 793800'
#TrackingRef '- Os(salen)binuclear.Dalton(CIF).cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C81.75 H80 Cl3.50 F12 N8 O4.25 Os2 P4'
_chemical_formula_weight         2098.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -4.9801 6.2216 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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'

_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                   21.63349(15)
_cell_length_b                   23.90315(17)
_cell_length_c                   15.89060(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.6675(8)
_cell_angle_gamma                90.00
_cell_volume                     8216.61(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    41251
_cell_measurement_theta_min      3.4327
_cell_measurement_theta_max      71.4822

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4160
_exptl_absorpt_coefficient_mu    8.247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.42124
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro, Oxford Diffraction Ltd'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.1270
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            59907
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.70
_diffrn_reflns_theta_max         67.00
_reflns_number_total             13910
_reflns_number_gt                12153
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep-3
_computing_publication_material  Wingx

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0333P)^2^+36.9282P] where P=(Fo^2^+2Fc^2^)/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         13910
_refine_ls_number_parameters     1103
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0889
_refine_ls_wR_factor_gt          0.0861
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.206472(9) -0.037266(8) 0.222876(13) 0.02223(6) Uani 1 1 d . . .
Os2 Os 0.369627(9) 0.076047(8) -0.105898(14) 0.02355(6) Uani 1 1 d . A .
P1 P 0.13864(6) -0.11876(5) 0.36773(8) 0.0299(3) Uani 1 1 d . . .
P2 P 0.47098(5) 0.10694(5) -0.25640(8) 0.0220(2) Uani 1 1 d . A .
P3 P 0.34151(8) 0.20322(6) 0.24597(10) 0.0446(4) Uani 1 1 d . . .
P4 P 0.07852(7) 0.01389(8) 0.83675(10) 0.0444(4) Uani 1 1 d . . .
F1 F 0.4076(3) 0.1784(2) 0.2318(4) 0.127(3) Uani 1 1 d . . .
F2 F 0.3529(3) 0.24302(19) 0.1679(3) 0.0904(16) Uani 1 1 d . . .
F3 F 0.3717(2) 0.2493(2) 0.3063(3) 0.0940(17) Uani 1 1 d . . .
F4 F 0.3326(3) 0.1655(3) 0.3258(3) 0.1067(19) Uani 1 1 d . . .
F5 F 0.3122(4) 0.1577(2) 0.1874(3) 0.122(2) Uani 1 1 d . . .
F6 F 0.27615(19) 0.2287(2) 0.2594(3) 0.0828(15) Uani 1 1 d . . .
F7 F 0.0839(3) -0.0484(2) 0.8088(4) 0.111(2) Uani 1 1 d . . .
F8 F 0.1129(2) 0.0361(3) 0.7562(3) 0.118(3) Uani 1 1 d . . .
F9 F 0.01451(15) 0.01731(17) 0.7851(2) 0.0546(10) Uani 1 1 d . . .
F10 F 0.04278(19) -0.0033(2) 0.9185(3) 0.0756(13) Uani 1 1 d . . .
F11 F 0.14223(17) 0.0107(2) 0.8868(3) 0.0757(14) Uani 1 1 d . . .
F12 F 0.0713(3) 0.0771(2) 0.8658(4) 0.0957(17) Uani 1 1 d . . .
O2 O 0.20209(14) -0.11586(13) 0.17591(19) 0.0218(7) Uani 1 1 d . . .
O1 O 0.28107(15) -0.05904(14) 0.2927(2) 0.0268(7) Uani 1 1 d . . .
O4 O 0.37575(15) 0.00211(13) -0.1655(2) 0.0261(7) Uani 1 1 d . . .
O3 O 0.45486(14) 0.06342(13) -0.0553(2) 0.0246(7) Uani 1 1 d . . .
N2 N 0.13508(17) -0.01018(16) 0.1530(3) 0.0244(9) Uani 1 1 d . . .
N1 N 0.20555(19) 0.04061(17) 0.2680(3) 0.0279(9) Uani 1 1 d . . .
N5 N 0.1500(2) -0.05984(18) 0.3214(3) 0.0315(10) Uani 1 1 d . . .
H5N H 0.1281 -0.0320 0.3417 0.038 Uiso 1 1 calc R . .
N7 N 0.26469(17) -0.01297(16) 0.1268(3) 0.0239(8) Uani 1 1 d . A .
N4 N 0.28556(18) 0.09241(18) -0.1531(3) 0.0307(10) Uani 1 1 d . . .
N3 N 0.35708(19) 0.14844(17) -0.0459(3) 0.0283(9) Uani 1 1 d . . .
N6 N 0.40665(18) 0.11626(16) -0.2082(3) 0.0263(9) Uani 1 1 d . . .
H6N H 0.3834 0.1431 -0.2292 0.032 Uiso 1 1 calc R A .
N8 N 0.33047(18) 0.03402(16) -0.0062(3) 0.0257(9) Uani 1 1 d . . .
C20 C 0.1609(2) -0.1330(2) 0.1191(3) 0.0252(10) Uani 1 1 d . . .
C19 C 0.1625(2) -0.1897(2) 0.0961(3) 0.0317(12) Uani 1 1 d . . .
H19A H 0.1926 -0.2134 0.1215 0.038 Uiso 1 1 calc R . .
C18 C 0.1220(3) -0.2120(2) 0.0382(4) 0.0446(15) Uani 1 1 d . . .
H18A H 0.1247 -0.2505 0.0238 0.053 Uiso 1 1 calc R . .
C17 C 0.0771(3) -0.1787(3) 0.0005(4) 0.0511(17) Uani 1 1 d . . .
H17A H 0.0489 -0.1941 -0.0394 0.061 Uiso 1 1 calc R . .
C16 C 0.0739(3) -0.1232(3) 0.0214(4) 0.0448(15) Uani 1 1 d . . .
H16A H 0.0433 -0.1006 -0.0050 0.054 Uiso 1 1 calc R . .
C15 C 0.1146(2) -0.0983(2) 0.0814(3) 0.0272(11) Uani 1 1 d . . .
C14 C 0.1042(2) -0.0400(2) 0.0995(3) 0.0284(11) Uani 1 1 d . . .
H14A H 0.0718 -0.0219 0.0693 0.034 Uiso 1 1 calc R . .
C13 C 0.1180(3) 0.0488(2) 0.1725(5) 0.0502(17) Uani 1 1 d . . .
H13A H 0.0868 0.0448 0.2181 0.060 Uiso 1 1 calc R . .
C12 C 0.0844(3) 0.0811(2) 0.1068(4) 0.0471(16) Uani 1 1 d . . .
H12A H 0.0455 0.0615 0.0921 0.057 Uiso 1 1 calc R . .
H12B H 0.1099 0.0828 0.0556 0.057 Uiso 1 1 calc R . .
C11 C 0.0695(3) 0.1401(3) 0.1351(6) 0.069(2) Uani 1 1 d . . .
H11A H 0.0604 0.1629 0.0844 0.083 Uiso 1 1 calc R . .
H11B H 0.0311 0.1387 0.1685 0.083 Uiso 1 1 calc R . .
C10 C 0.1165(4) 0.1694(3) 0.1849(6) 0.077(3) Uani 1 1 d . . .
H10A H 0.0962 0.2008 0.2144 0.093 Uiso 1 1 calc R . .
H10B H 0.1468 0.1857 0.1458 0.093 Uiso 1 1 calc R . .
C9 C 0.1515(3) 0.1351(2) 0.2498(4) 0.0436(14) Uani 1 1 d . . .
H9A H 0.1894 0.1553 0.2675 0.052 Uiso 1 1 calc R . .
H9B H 0.1256 0.1296 0.3000 0.052 Uiso 1 1 calc R . .
C8 C 0.1688(3) 0.0792(2) 0.2140(5) 0.0546(18) Uani 1 1 d . . .
H8A H 0.1974 0.0886 0.1669 0.066 Uiso 1 1 calc R . .
C7 C 0.2381(2) 0.0582(2) 0.3319(3) 0.0316(12) Uani 1 1 d . . .
H7A H 0.2332 0.0961 0.3483 0.038 Uiso 1 1 calc R . .
C6 C 0.2808(2) 0.0246(2) 0.3797(3) 0.0328(12) Uani 1 1 d . . .
C5 C 0.3075(3) 0.0503(3) 0.4529(4) 0.0465(15) Uani 1 1 d . . .
H5A H 0.2952 0.0872 0.4675 0.056 Uiso 1 1 calc R . .
C4 C 0.3497(3) 0.0237(3) 0.5020(4) 0.0519(17) Uani 1 1 d . . .
H4A H 0.3670 0.0417 0.5501 0.062 Uiso 1 1 calc R . .
C3 C 0.3676(3) -0.0306(3) 0.4809(4) 0.0440(15) Uani 1 1 d . . .
H3A H 0.3971 -0.0495 0.5152 0.053 Uiso 1 1 calc R . .
C2 C 0.3435(2) -0.0568(2) 0.4118(3) 0.0335(12) Uani 1 1 d . . .
H2A H 0.3566 -0.0938 0.3990 0.040 Uiso 1 1 calc R . .
C1 C 0.2998(2) -0.0307(2) 0.3594(3) 0.0271(11) Uani 1 1 d . . .
C41 C 0.2079(2) -0.1565(2) 0.3974(3) 0.0311(11) Uani 1 1 d . . .
C42 C 0.2459(2) -0.1793(2) 0.3375(3) 0.0322(12) Uani 1 1 d . . .
H42A H 0.2366 -0.1739 0.2795 0.039 Uiso 1 1 calc R . .
C43 C 0.2976(3) -0.2101(2) 0.3610(4) 0.0353(12) Uani 1 1 d . . .
H43A H 0.3235 -0.2257 0.3193 0.042 Uiso 1 1 calc R . .
C44 C 0.3113(3) -0.2181(2) 0.4451(4) 0.0379(13) Uani 1 1 d . . .
H44A H 0.3464 -0.2396 0.4613 0.046 Uiso 1 1 calc R . .
C45 C 0.2742(3) -0.1950(2) 0.5054(4) 0.0386(13) Uani 1 1 d . . .
H45A H 0.2843 -0.2002 0.5632 0.046 Uiso 1 1 calc R . .
C46 C 0.2225(3) -0.1644(2) 0.4832(3) 0.0337(12) Uani 1 1 d . . .
H46A H 0.1970 -0.1487 0.5254 0.040 Uiso 1 1 calc R . .
C47 C 0.0973(3) -0.1038(3) 0.4632(4) 0.0392(13) Uani 1 1 d . . .
C52 C 0.0518(3) -0.1402(3) 0.4911(4) 0.0521(16) Uani 1 1 d . . .
H52A H 0.0412 -0.1726 0.4595 0.063 Uiso 1 1 calc R . .
C51 C 0.0220(4) -0.1283(4) 0.5665(5) 0.073(2) Uani 1 1 d . . .
H51A H -0.0085 -0.1532 0.5870 0.087 Uiso 1 1 calc R . .
C50 C 0.0366(4) -0.0810(4) 0.6111(5) 0.074(2) Uani 1 1 d . . .
H50A H 0.0156 -0.0732 0.6620 0.089 Uiso 1 1 calc R . .
C49 C 0.0809(4) -0.0446(4) 0.5836(5) 0.067(2) Uani 1 1 d . . .
H49A H 0.0908 -0.0120 0.6152 0.080 Uiso 1 1 calc R . .
C48 C 0.1112(3) -0.0560(3) 0.5090(4) 0.0543(17) Uani 1 1 d . . .
H48A H 0.1417 -0.0308 0.4891 0.065 Uiso 1 1 calc R . .
C53 C 0.0917(2) -0.1669(2) 0.3078(3) 0.0337(12) Uani 1 1 d . . .
C54 C 0.0456(3) -0.1444(3) 0.2561(4) 0.0432(14) Uani 1 1 d . . .
H54A H 0.0410 -0.1050 0.2512 0.052 Uiso 1 1 calc R . .
C55 C 0.0066(3) -0.1798(3) 0.2122(4) 0.0565(18) Uani 1 1 d . . .
H55A H -0.0250 -0.1647 0.1768 0.068 Uiso 1 1 calc R . .
C56 C 0.0132(3) -0.2375(3) 0.2194(4) 0.0596(19) Uani 1 1 d . . .
H56A H -0.0141 -0.2617 0.1895 0.072 Uiso 1 1 calc R . .
C57 C 0.0592(3) -0.2594(3) 0.2699(5) 0.0525(17) Uani 1 1 d . . .
H57A H 0.0639 -0.2989 0.2741 0.063 Uiso 1 1 calc R . .
C58 C 0.0986(3) -0.2247(2) 0.3144(4) 0.0409(14) Uani 1 1 d . . .
H58A H 0.1302 -0.2401 0.3494 0.049 Uiso 1 1 calc R . .
C40 C 0.3390(2) -0.0127(2) -0.2286(3) 0.0304(11) Uani 1 1 d . . .
C39 C 0.3556(3) -0.0615(2) -0.2733(4) 0.0373(13) Uani 1 1 d . . .
H39A H 0.3916 -0.0815 -0.2568 0.045 Uiso 1 1 calc R . .
C38 C 0.3206(3) -0.0805(3) -0.3402(4) 0.0516(16) Uani 1 1 d . . .
H38A H 0.3332 -0.1130 -0.3701 0.062 Uiso 1 1 calc R . .
C37 C 0.2661(3) -0.0522(3) -0.3648(5) 0.0597(19) Uani 1 1 d . . .
H37A H 0.2415 -0.0658 -0.4103 0.072 Uiso 1 1 calc R . .
C36 C 0.2495(3) -0.0057(3) -0.3228(4) 0.0539(17) Uani 1 1 d . . .
H36A H 0.2129 0.0132 -0.3401 0.065 Uiso 1 1 calc R . .
C35 C 0.2839(2) 0.0164(2) -0.2538(4) 0.0364(13) Uani 1 1 d . . .
C34 C 0.2591(2) 0.0649(2) -0.2133(4) 0.0359(13) Uani 1 1 d . . .
H34A H 0.2199 0.0778 -0.2324 0.043 Uiso 1 1 calc R . .
C28A C 0.2986(5) 0.1775(4) -0.0738(7) 0.033(2) Uani 0.60 1 d PDU A 1
H28A H 0.3088 0.2008 -0.1240 0.039 Uiso 0.60 1 calc PR A 1
C29A C 0.2697(7) 0.2159(6) -0.0091(11) 0.044(3) Uani 0.60 1 d PDU A 1
H29A H 0.3000 0.2446 0.0092 0.053 Uiso 0.60 1 calc PR A 1
H29B H 0.2572 0.1941 0.0408 0.053 Uiso 0.60 1 calc PR A 1
C30A C 0.2129(7) 0.2441(6) -0.0497(9) 0.055(4) Uani 0.60 1 d PDU A 1
H30A H 0.1928 0.2686 -0.0078 0.067 Uiso 0.60 1 calc PR A 1
H30B H 0.2263 0.2679 -0.0971 0.067 Uiso 0.60 1 calc PR A 1
C31A C 0.1672(7) 0.2019(6) -0.0813(10) 0.057(4) Uani 0.60 1 d PDU A 1
H31A H 0.1312 0.2216 -0.1063 0.069 Uiso 0.60 1 calc PR A 1
H31B H 0.1524 0.1794 -0.0334 0.069 Uiso 0.60 1 calc PR A 1
C32A C 0.1956(6) 0.1620(6) -0.1489(8) 0.040(3) Uani 0.60 1 d PDU A 1
H32A H 0.1651 0.1336 -0.1676 0.048 Uiso 0.60 1 calc PR A 1
H32B H 0.2097 0.1833 -0.1985 0.048 Uiso 0.60 1 calc PR A 1
C33A C 0.2511(4) 0.1341(4) -0.1020(7) 0.034(2) Uani 0.60 1 d PDU A 1
H33A H 0.2351 0.1148 -0.0509 0.040 Uiso 0.60 1 calc PR A 1
C28B C 0.2917(10) 0.1665(7) -0.0428(11) 0.039(4) Uani 0.40 1 d PDU A 2
H28B H 0.2711 0.1427 0.0003 0.047 Uiso 0.40 1 calc PR A 2
C29B C 0.2767(11) 0.2269(9) -0.0216(19) 0.045(5) Uani 0.40 1 d PDU A 2
H29C H 0.2956 0.2520 -0.0637 0.053 Uiso 0.40 1 calc PR A 2
H29D H 0.2946 0.2363 0.0343 0.053 Uiso 0.40 1 calc PR A 2
C30B C 0.2067(9) 0.2366(10) -0.0206(13) 0.050(5) Uani 0.40 1 d PDU A 2
H30C H 0.1986 0.2771 -0.0135 0.060 Uiso 0.40 1 calc PR A 2
H30D H 0.1892 0.2169 0.0285 0.060 Uiso 0.40 1 calc PR A 2
C31B C 0.1738(12) 0.2161(8) -0.1010(15) 0.058(5) Uani 0.40 1 d PDU A 2
H31C H 0.1285 0.2169 -0.0930 0.069 Uiso 0.40 1 calc PR A 2
H31D H 0.1838 0.2412 -0.1485 0.069 Uiso 0.40 1 calc PR A 2
C32B C 0.1943(9) 0.1565(9) -0.1215(15) 0.049(5) Uani 0.40 1 d PDU A 2
H32C H 0.1794 0.1311 -0.0770 0.058 Uiso 0.40 1 calc PR A 2
H32D H 0.1748 0.1449 -0.1753 0.058 Uiso 0.40 1 calc PR A 2
C33B C 0.2640(8) 0.1503(7) -0.1285(11) 0.042(4) Uani 0.40 1 d PDU A 2
H33B H 0.2790 0.1775 -0.1715 0.051 Uiso 0.40 1 calc PR A 2
C27 C 0.3979(2) 0.17230(19) 0.0038(3) 0.0279(11) Uani 1 1 d . A .
H27A H 0.3866 0.2069 0.0286 0.033 Uiso 1 1 calc R . .
C26 C 0.4581(2) 0.1508(2) 0.0240(3) 0.0291(11) Uani 1 1 d . . .
C25 C 0.4949(3) 0.1849(2) 0.0778(3) 0.0362(13) Uani 1 1 d . A .
H25A H 0.4784 0.2194 0.0970 0.043 Uiso 1 1 calc R . .
C24 C 0.5532(3) 0.1697(2) 0.1028(4) 0.0396(13) Uani 1 1 d . . .
H24A H 0.5767 0.1932 0.1393 0.048 Uiso 1 1 calc R A .
C23 C 0.5779(3) 0.1190(2) 0.0739(3) 0.0342(12) Uani 1 1 d . A .
H23A H 0.6186 0.1084 0.0902 0.041 Uiso 1 1 calc R . .
C22 C 0.5433(2) 0.0847(2) 0.0221(3) 0.0295(11) Uani 1 1 d . . .
H22A H 0.5604 0.0501 0.0043 0.035 Uiso 1 1 calc R A .
C21 C 0.4837(2) 0.09946(19) -0.0050(3) 0.0256(10) Uani 1 1 d . A .
C71 C 0.4904(2) 0.03481(19) -0.2764(3) 0.0240(10) Uani 1 1 d . . .
C76 C 0.5079(2) -0.0011(2) -0.2112(3) 0.0264(10) Uani 1 1 d . A .
H76A H 0.5072 0.0116 -0.1546 0.032 Uiso 1 1 calc R . .
C75 C 0.5263(2) -0.0550(2) -0.2290(3) 0.0299(11) Uani 1 1 d . . .
H75A H 0.5374 -0.0796 -0.1843 0.036 Uiso 1 1 calc R A .
C74 C 0.5285(3) -0.0739(2) -0.3121(3) 0.0346(12) Uani 1 1 d . A .
H74A H 0.5422 -0.1107 -0.3242 0.041 Uiso 1 1 calc R . .
C73 C 0.5109(3) -0.0388(2) -0.3761(4) 0.0388(13) Uani 1 1 d . . .
H73A H 0.5118 -0.0516 -0.4326 0.047 Uiso 1 1 calc R A .
C72 C 0.4916(2) 0.0154(2) -0.3591(3) 0.0308(11) Uani 1 1 d . A .
H72A H 0.4791 0.0394 -0.4039 0.037 Uiso 1 1 calc R . .
C65 C 0.4664(2) 0.14050(19) -0.3577(3) 0.0259(10) Uani 1 1 d . . .
C66 C 0.4098(3) 0.1476(2) -0.3992(3) 0.0330(12) Uani 1 1 d . A .
H66A H 0.3723 0.1386 -0.3717 0.040 Uiso 1 1 calc R . .
C67 C 0.4085(3) 0.1680(2) -0.4815(4) 0.0391(14) Uani 1 1 d . . .
H67A H 0.3701 0.1734 -0.5098 0.047 Uiso 1 1 calc R A .
C68 C 0.4627(3) 0.1803(2) -0.5216(3) 0.0402(14) Uani 1 1 d . A .
H68A H 0.4614 0.1938 -0.5778 0.048 Uiso 1 1 calc R . .
C69 C 0.5181(3) 0.1734(2) -0.4818(4) 0.0427(14) Uani 1 1 d . . .
H69A H 0.5553 0.1816 -0.5105 0.051 Uiso 1 1 calc R A .
C70 C 0.5205(3) 0.1543(2) -0.3992(3) 0.0332(12) Uani 1 1 d . A .
H70A H 0.5592 0.1506 -0.3710 0.040 Uiso 1 1 calc R . .
C59 C 0.5370(2) 0.1374(2) -0.2038(3) 0.0258(10) Uani 1 1 d . . .
C60 C 0.5951(2) 0.1129(2) -0.2038(3) 0.0276(11) Uani 1 1 d . A .
H60A H 0.6008 0.0774 -0.2296 0.033 Uiso 1 1 calc R . .
C61 C 0.6449(2) 0.1399(2) -0.1663(3) 0.0351(12) Uani 1 1 d . . .
H61A H 0.6846 0.1227 -0.1660 0.042 Uiso 1 1 calc R A .
C62 C 0.6374(3) 0.1908(3) -0.1300(4) 0.0537(18) Uani 1 1 d . A .
H62A H 0.6718 0.2094 -0.1051 0.064 Uiso 1 1 calc R . .
C63 C 0.5797(3) 0.2153(3) -0.1291(5) 0.071(2) Uani 1 1 d . . .
H63A H 0.5746 0.2507 -0.1029 0.085 Uiso 1 1 calc R A .
C64 C 0.5290(3) 0.1888(3) -0.1663(4) 0.0491(17) Uani 1 1 d . A .
H64A H 0.4894 0.2060 -0.1658 0.059 Uiso 1 1 calc R . .
C77 C 0.2533(2) -0.0270(2) 0.0452(3) 0.0275(11) Uani 1 1 d . . .
H77A H 0.2217 -0.0535 0.0328 0.033 Uiso 1 1 calc R A .
C78 C 0.2856(2) -0.0041(2) -0.0196(3) 0.0276(11) Uani 1 1 d . A .
H78A H 0.2762 -0.0154 -0.0756 0.033 Uiso 1 1 calc R . .
C79 C 0.3446(2) 0.0454(2) 0.0750(3) 0.0275(11) Uani 1 1 d . A .
H79A H 0.3778 0.0702 0.0872 0.033 Uiso 1 1 calc R . .
C80 C 0.3129(2) 0.0225(2) 0.1400(3) 0.0266(11) Uani 1 1 d . . .
H80A H 0.3248 0.0315 0.1961 0.032 Uiso 1 1 calc R A .
C1S C 0.2047(4) 0.8761(3) 0.8047(5) 0.069(2) Uani 1 1 d . . .
H1SA H 0.2266 0.9092 0.7825 0.082 Uiso 1 1 calc R . .
H1SB H 0.1616 0.8873 0.8164 0.082 Uiso 1 1 calc R . .
Cl1 Cl 0.23975(14) 0.85563(9) 0.89711(13) 0.0911(8) Uani 1 1 d . . .
Cl2 Cl 0.20401(11) 0.82316(8) 0.72734(13) 0.0759(6) Uani 1 1 d . . .
C2S C 0.1028(8) 0.1300(8) 0.6095(9) 0.140(8) Uani 0.75 1 d P B 1
H2S1 H 0.0643 0.1078 0.6138 0.168 Uiso 0.75 1 calc PR B 1
H2S2 H 0.1245 0.1277 0.6646 0.168 Uiso 0.75 1 calc PR B 1
Cl3 Cl 0.14884(14) 0.10000(12) 0.5342(3) 0.0946(11) Uani 0.75 1 d P B 1
Cl4 Cl 0.08367(17) 0.19746(17) 0.5912(3) 0.1373(19) Uani 0.75 1 d P B 1
O1W O 0.1860(7) 0.1804(6) 0.6543(10) 0.041(4) Uiso 0.25 1 d P C 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os1 0.02257(11) 0.02155(10) 0.02266(12) 0.00198(8) 0.00370(9) -0.00019(8)
Os2 0.02242(11) 0.02225(10) 0.02615(12) 0.00380(8) 0.00722(9) 0.00073(8)
P1 0.0316(7) 0.0314(7) 0.0268(7) 0.0070(5) 0.0089(6) 0.0023(5)
P2 0.0220(6) 0.0227(6) 0.0213(6) 0.0016(5) 0.0040(5) 0.0003(4)
P3 0.0655(10) 0.0325(7) 0.0364(8) -0.0017(6) 0.0173(8) 0.0026(7)
P4 0.0289(7) 0.0639(10) 0.0406(9) 0.0078(8) 0.0059(7) -0.0004(7)
F1 0.128(5) 0.104(4) 0.150(6) 0.050(4) 0.084(4) 0.068(4)
F2 0.129(4) 0.058(3) 0.085(3) 0.032(2) 0.021(3) 0.005(3)
F3 0.060(3) 0.127(4) 0.096(4) -0.044(3) 0.007(3) -0.029(3)
F4 0.125(5) 0.125(5) 0.070(3) 0.049(3) 0.015(3) -0.026(4)
F5 0.223(7) 0.062(3) 0.082(4) -0.041(3) 0.034(4) -0.038(4)
F6 0.050(2) 0.101(4) 0.097(4) -0.037(3) -0.011(2) 0.007(2)
F7 0.115(4) 0.093(4) 0.125(5) -0.044(3) -0.055(4) 0.059(3)
F8 0.057(3) 0.248(8) 0.051(3) 0.032(4) 0.008(2) -0.055(4)
F9 0.0357(18) 0.072(2) 0.056(2) 0.0172(19) -0.0025(17) -0.0012(17)
F10 0.054(2) 0.120(4) 0.053(2) 0.025(3) 0.004(2) -0.023(2)
F11 0.038(2) 0.132(4) 0.056(3) 0.002(3) -0.0069(19) 0.005(2)
F12 0.109(4) 0.068(3) 0.110(4) -0.004(3) -0.030(3) -0.007(3)
O2 0.0230(16) 0.0221(16) 0.0202(16) 0.0011(13) -0.0024(14) -0.0011(13)
O1 0.0243(17) 0.0312(18) 0.0248(18) -0.0035(14) -0.0024(15) 0.0041(14)
O4 0.0249(16) 0.0242(16) 0.0292(19) 0.0002(14) -0.0019(15) -0.0026(13)
O3 0.0228(16) 0.0239(16) 0.0272(18) -0.0022(14) 0.0035(14) 0.0024(13)
N2 0.0207(19) 0.024(2) 0.029(2) 0.0033(17) 0.0019(18) 0.0032(16)
N1 0.031(2) 0.024(2) 0.028(2) -0.0031(18) 0.0031(19) 0.0016(17)
N5 0.031(2) 0.030(2) 0.033(2) 0.0025(19) 0.015(2) 0.0061(18)
N7 0.0207(19) 0.027(2) 0.025(2) 0.0007(17) 0.0079(17) -0.0011(16)
N4 0.0174(19) 0.036(2) 0.039(3) 0.009(2) 0.0054(19) 0.0022(17)
N3 0.029(2) 0.024(2) 0.032(2) 0.0050(18) 0.0145(19) 0.0035(17)
N6 0.029(2) 0.024(2) 0.026(2) 0.0072(17) 0.0030(18) 0.0051(16)
N8 0.026(2) 0.023(2) 0.028(2) 0.0031(17) 0.0072(18) 0.0012(16)
C20 0.027(2) 0.029(2) 0.019(2) 0.005(2) 0.002(2) 0.000(2)
C19 0.036(3) 0.030(3) 0.029(3) 0.000(2) -0.001(2) 0.006(2)
C18 0.053(4) 0.036(3) 0.044(4) -0.010(3) -0.014(3) 0.008(3)
C17 0.058(4) 0.043(3) 0.051(4) -0.015(3) -0.029(3) 0.008(3)
C16 0.049(3) 0.040(3) 0.045(4) -0.005(3) -0.004(3) 0.003(3)
C15 0.026(2) 0.031(3) 0.025(3) 0.002(2) -0.003(2) 0.000(2)
C14 0.028(3) 0.032(3) 0.026(3) 0.006(2) -0.001(2) 0.004(2)
C13 0.048(4) 0.025(3) 0.077(5) -0.004(3) -0.017(3) 0.006(2)
C12 0.043(3) 0.030(3) 0.068(4) 0.006(3) -0.014(3) 0.005(2)
C11 0.057(4) 0.032(3) 0.117(7) 0.000(4) -0.025(4) 0.014(3)
C10 0.087(6) 0.035(4) 0.109(7) -0.011(4) -0.025(5) 0.020(4)
C9 0.041(3) 0.027(3) 0.063(4) -0.003(3) 0.006(3) 0.004(2)
C8 0.068(4) 0.031(3) 0.065(4) -0.010(3) -0.018(4) 0.013(3)
C7 0.036(3) 0.025(2) 0.034(3) -0.005(2) 0.006(2) 0.001(2)
C6 0.035(3) 0.031(3) 0.032(3) -0.002(2) 0.002(2) -0.005(2)
C5 0.058(4) 0.035(3) 0.046(4) -0.011(3) -0.007(3) -0.007(3)
C4 0.063(4) 0.047(4) 0.045(4) -0.010(3) -0.019(3) -0.005(3)
C3 0.045(3) 0.046(3) 0.041(3) 0.004(3) -0.012(3) -0.006(3)
C2 0.033(3) 0.033(3) 0.034(3) 0.000(2) 0.001(2) -0.004(2)
C1 0.027(2) 0.032(3) 0.022(3) -0.001(2) 0.005(2) -0.006(2)
C41 0.032(3) 0.027(3) 0.035(3) 0.005(2) 0.007(2) -0.002(2)
C42 0.035(3) 0.033(3) 0.028(3) 0.007(2) 0.002(2) 0.002(2)
C43 0.034(3) 0.034(3) 0.038(3) 0.004(2) 0.002(3) 0.006(2)
C44 0.038(3) 0.031(3) 0.044(3) 0.003(2) -0.006(3) -0.001(2)
C45 0.049(3) 0.035(3) 0.031(3) 0.001(2) -0.008(3) -0.003(3)
C46 0.044(3) 0.030(3) 0.028(3) 0.001(2) 0.004(3) -0.003(2)
C47 0.039(3) 0.048(3) 0.030(3) 0.010(3) 0.010(3) 0.008(3)
C52 0.053(4) 0.063(4) 0.042(4) 0.013(3) 0.017(3) 0.003(3)
C51 0.072(5) 0.100(7) 0.048(4) 0.017(4) 0.025(4) -0.019(5)
C50 0.070(5) 0.113(7) 0.039(4) -0.001(5) 0.028(4) 0.006(5)
C49 0.067(5) 0.091(6) 0.043(4) -0.021(4) 0.020(4) 0.001(4)
C48 0.055(4) 0.064(4) 0.044(4) -0.008(3) 0.015(3) 0.000(3)
C53 0.031(3) 0.040(3) 0.030(3) 0.005(2) 0.008(2) 0.000(2)
C54 0.035(3) 0.058(4) 0.037(3) 0.006(3) 0.004(3) 0.003(3)
C55 0.039(3) 0.084(5) 0.046(4) -0.001(4) -0.004(3) 0.007(3)
C56 0.044(4) 0.083(5) 0.052(4) -0.020(4) 0.002(3) -0.014(4)
C57 0.041(3) 0.047(4) 0.069(5) -0.007(3) 0.005(3) -0.005(3)
C58 0.038(3) 0.042(3) 0.044(4) 0.001(3) 0.008(3) -0.003(2)
C40 0.029(3) 0.037(3) 0.025(3) 0.004(2) 0.005(2) -0.008(2)
C39 0.040(3) 0.037(3) 0.034(3) -0.002(2) 0.001(3) -0.006(2)
C38 0.054(4) 0.052(4) 0.049(4) -0.014(3) -0.005(3) -0.008(3)
C37 0.052(4) 0.071(5) 0.055(4) -0.013(4) -0.017(4) -0.011(3)
C36 0.052(4) 0.063(4) 0.046(4) -0.001(3) -0.001(3) -0.006(3)
C35 0.026(3) 0.045(3) 0.038(3) 0.009(3) -0.003(2) -0.007(2)
C34 0.021(2) 0.045(3) 0.041(3) 0.014(3) 0.001(2) 0.001(2)
C28A 0.030(4) 0.034(5) 0.034(5) 0.010(4) 0.016(4) 0.011(3)
C29A 0.046(5) 0.034(6) 0.052(7) 0.005(5) 0.024(4) 0.012(4)
C30A 0.058(6) 0.051(6) 0.058(7) 0.003(5) 0.020(6) 0.028(4)
C31A 0.045(5) 0.054(6) 0.074(7) 0.015(5) 0.015(5) 0.026(4)
C32A 0.031(4) 0.043(5) 0.046(6) 0.018(4) 0.009(4) 0.008(4)
C33A 0.028(4) 0.034(5) 0.040(5) 0.013(4) 0.016(4) 0.009(3)
C28B 0.042(7) 0.035(6) 0.039(7) 0.009(6) 0.015(6) 0.008(5)
C29B 0.047(6) 0.040(7) 0.047(9) 0.004(6) 0.014(6) 0.012(7)
C30B 0.049(7) 0.044(7) 0.058(9) 0.009(7) 0.026(7) 0.014(6)
C31B 0.047(7) 0.047(8) 0.079(9) 0.011(8) 0.007(7) 0.008(6)
C32B 0.043(6) 0.045(7) 0.058(10) 0.012(7) 0.009(6) 0.003(6)
C33B 0.041(6) 0.036(7) 0.049(7) 0.009(6) 0.004(6) 0.001(5)
C27 0.037(3) 0.019(2) 0.028(3) 0.001(2) 0.015(2) 0.000(2)
C26 0.041(3) 0.025(2) 0.022(3) 0.001(2) 0.012(2) -0.002(2)
C25 0.050(3) 0.029(3) 0.029(3) -0.003(2) 0.013(3) -0.006(2)
C24 0.055(4) 0.034(3) 0.030(3) -0.002(2) 0.002(3) -0.012(3)
C23 0.035(3) 0.040(3) 0.027(3) 0.001(2) 0.002(2) -0.006(2)
C22 0.034(3) 0.029(3) 0.026(3) -0.001(2) 0.007(2) 0.000(2)
C21 0.030(3) 0.023(2) 0.024(3) 0.0047(19) 0.006(2) -0.0030(19)
C71 0.022(2) 0.023(2) 0.027(3) 0.000(2) 0.006(2) 0.0008(18)
C76 0.027(2) 0.029(2) 0.024(3) -0.003(2) 0.003(2) -0.002(2)
C75 0.033(3) 0.027(2) 0.031(3) 0.002(2) 0.000(2) 0.002(2)
C74 0.043(3) 0.026(3) 0.035(3) -0.005(2) 0.005(3) 0.004(2)
C73 0.053(3) 0.034(3) 0.029(3) -0.006(2) 0.007(3) 0.002(3)
C72 0.039(3) 0.031(3) 0.023(3) 0.000(2) 0.000(2) -0.001(2)
C65 0.035(3) 0.018(2) 0.024(3) -0.0002(19) 0.004(2) -0.0009(19)
C66 0.037(3) 0.029(3) 0.033(3) 0.003(2) -0.001(2) -0.001(2)
C67 0.050(3) 0.024(3) 0.043(3) 0.004(2) -0.012(3) 0.002(2)
C68 0.073(4) 0.024(3) 0.023(3) 0.002(2) 0.001(3) -0.002(3)
C69 0.054(4) 0.040(3) 0.035(3) 0.005(3) 0.018(3) 0.002(3)
C70 0.037(3) 0.033(3) 0.030(3) 0.006(2) 0.009(2) -0.003(2)
C59 0.027(2) 0.031(3) 0.020(2) -0.005(2) 0.004(2) -0.001(2)
C60 0.026(2) 0.029(2) 0.028(3) -0.004(2) 0.004(2) 0.001(2)
C61 0.026(3) 0.048(3) 0.032(3) -0.006(2) 0.002(2) -0.002(2)
C62 0.032(3) 0.067(4) 0.062(4) -0.033(4) 0.003(3) -0.011(3)
C63 0.050(4) 0.059(4) 0.103(6) -0.060(4) 0.000(4) -0.002(3)
C64 0.026(3) 0.047(3) 0.075(5) -0.028(3) 0.002(3) 0.003(2)
C77 0.028(2) 0.027(2) 0.028(3) 0.001(2) 0.003(2) -0.004(2)
C78 0.030(3) 0.027(2) 0.026(3) 0.000(2) 0.003(2) 0.000(2)
C79 0.026(2) 0.026(2) 0.031(3) 0.005(2) 0.004(2) -0.0031(19)
C80 0.024(2) 0.029(2) 0.028(3) 0.002(2) 0.002(2) -0.0018(19)
C1S 0.080(5) 0.046(4) 0.079(6) -0.005(4) -0.006(4) 0.006(4)
Cl1 0.155(2) 0.0591(11) 0.0585(12) -0.0093(9) -0.0145(13) 0.0275(13)
Cl2 0.1015(15) 0.0624(11) 0.0638(12) -0.0082(9) -0.0002(11) -0.0300(11)
C2S 0.166(16) 0.164(16) 0.092(10) 0.065(11) 0.056(11) 0.096(13)
Cl3 0.0765(18) 0.0670(17) 0.141(3) 0.0183(18) 0.048(2) 0.0117(14)
Cl4 0.100(2) 0.108(3) 0.206(5) -0.078(3) 0.090(3) -0.054(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
Os1 N1 1.995(4) . ?
Os1 N2 1.999(4) . ?
Os1 O1 2.016(3) . ?
Os1 O2 2.023(3) . ?
Os1 N5 2.068(4) . ?
Os1 N7 2.074(4) . ?
Os2 N3 1.996(4) . ?
Os2 N4 1.998(4) . ?
Os2 O4 2.010(3) . ?
Os2 O3 2.025(3) . ?
Os2 N6 2.058(4) . ?
Os2 N8 2.066(4) . ?
P1 N5 1.610(4) . ?
P1 C53 1.800(6) . ?
P1 C47 1.807(6) . ?
P1 C41 1.807(5) . ?
P2 N6 1.612(4) . ?
P2 C65 1.800(5) . ?
P2 C59 1.800(5) . ?
P2 C71 1.804(5) . ?
P3 F6 1.557(4) . ?
P3 F5 1.562(5) . ?
P3 F1 1.567(5) . ?
P3 F4 1.570(5) . ?
P3 F2 1.585(4) . ?
P3 F3 1.595(5) . ?
P4 F7 1.558(5) . ?
P4 F10 1.574(4) . ?
P4 F8 1.580(5) . ?
P4 F11 1.585(4) . ?
P4 F12 1.588(5) . ?
P4 F9 1.604(4) . ?
O2 C20 1.325(6) . ?
O1 C1 1.318(6) . ?
O4 C40 1.321(6) . ?
O3 C21 1.327(6) . ?
N2 C14 1.290(6) . ?
N2 C13 1.491(7) . ?
N1 C7 1.298(7) . ?
N1 C8 1.484(7) . ?
N5 H5N 0.8800 . ?
N7 C80 1.358(6) . ?
N7 C77 1.358(6) . ?
N4 C34 1.290(7) . ?
N4 C33A 1.490(11) . ?
N4 C33B 1.512(18) . ?
N3 C27 1.307(7) . ?
N3 C28B 1.48(2) . ?
N3 C28A 1.506(12) . ?
N6 H6N 0.8800 . ?
N8 C78 1.346(6) . ?
N8 C79 1.350(6) . ?
C20 C19 1.403(7) . ?
C20 C15 1.428(7) . ?
C19 C18 1.372(7) . ?
C19 H19A 0.9500 . ?
C18 C17 1.387(8) . ?
C18 H18A 0.9500 . ?
C17 C16 1.368(8) . ?
C17 H17A 0.9500 . ?
C16 C15 1.422(7) . ?
C16 H16A 0.9500 . ?
C15 C14 1.441(7) . ?
C14 H14A 0.9500 . ?
C13 C8 1.468(9) . ?
C13 C12 1.482(8) . ?
C13 H13A 1.0000 . ?
C12 C11 1.517(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C11 C10 1.459(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C10 C9 1.514(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C9 C8 1.501(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C8 H8A 1.0000 . ?
C7 C6 1.434(7) . ?
C7 H7A 0.9500 . ?
C6 C1 1.423(7) . ?
C6 C5 1.431(8) . ?
C5 C4 1.353(9) . ?
C5 H5A 0.9500 . ?
C4 C3 1.396(9) . ?
C4 H4A 0.9500 . ?
C3 C2 1.363(8) . ?
C3 H3A 0.9500 . ?
C2 C1 1.400(7) . ?
C2 H2A 0.9500 . ?
C41 C42 1.378(8) . ?
C41 C46 1.408(7) . ?
C42 C43 1.387(7) . ?
C42 H42A 0.9500 . ?
C43 C44 1.378(8) . ?
C43 H43A 0.9500 . ?
C44 C45 1.373(8) . ?
C44 H44A 0.9500 . ?
C45 C46 1.380(8) . ?
C45 H45A 0.9500 . ?
C46 H46A 0.9500 . ?
C47 C48 1.384(9) . ?
C47 C52 1.389(9) . ?
C52 C51 1.396(10) . ?
C52 H52A 0.9500 . ?
C51 C50 1.370(12) . ?
C51 H51A 0.9500 . ?
C50 C49 1.370(11) . ?
C50 H50A 0.9500 . ?
C49 C48 1.388(10) . ?
C49 H49A 0.9500 . ?
C48 H48A 0.9500 . ?
C53 C54 1.393(8) . ?
C53 C58 1.394(8) . ?
C54 C55 1.380(9) . ?
C54 H54A 0.9500 . ?
C55 C56 1.391(11) . ?
C55 H55A 0.9500 . ?
C56 C57 1.376(10) . ?
C56 H56A 0.9500 . ?
C57 C58 1.379(8) . ?
C57 H57A 0.9500 . ?
C58 H58A 0.9500 . ?
C40 C39 1.415(8) . ?
C40 C35 1.433(7) . ?
C39 C38 1.376(8) . ?
C39 H39A 0.9500 . ?
C38 C37 1.410(10) . ?
C38 H38A 0.9500 . ?
C37 C36 1.348(10) . ?
C37 H37A 0.9500 . ?
C36 C35 1.419(8) . ?
C36 H36A 0.9500 . ?
C35 C34 1.432(8) . ?
C34 H34A 0.9500 . ?
C28A C29A 1.519(14) . ?
C28A C33A 1.523(12) . ?
C28A H28A 1.0000 . ?
C29A C30A 1.538(15) . ?
C29A H29A 0.9900 . ?
C29A H29B 0.9900 . ?
C30A C31A 1.495(15) . ?
C30A H30A 0.9900 . ?
C30A H30B 0.9900 . ?
C31A C32A 1.568(14) . ?
C31A H31A 0.9900 . ?
C31A H31B 0.9900 . ?
C32A C33A 1.556(12) . ?
C32A H32A 0.9900 . ?
C32A H32B 0.9900 . ?
C33A H33A 1.0000 . ?
C28B C29B 1.519(17) . ?
C28B C33B 1.531(16) . ?
C28B H28B 1.0000 . ?
C29B C30B 1.531(18) . ?
C29B H29C 0.9900 . ?
C29B H29D 0.9900 . ?
C30B C31B 1.537(18) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C31B C32B 1.527(18) . ?
C31B H31C 0.9900 . ?
C31B H31D 0.9900 . ?
C32B C33B 1.520(17) . ?
C32B H32C 0.9900 . ?
C32B H32D 0.9900 . ?
C33B H33B 1.0000 . ?
C27 C26 1.435(7) . ?
C27 H27A 0.9500 . ?
C26 C25 1.418(7) . ?
C26 C21 1.424(7) . ?
C25 C24 1.367(8) . ?
C25 H25A 0.9500 . ?
C24 C23 1.403(8) . ?
C24 H24A 0.9500 . ?
C23 C22 1.377(7) . ?
C23 H23A 0.9500 . ?
C22 C21 1.400(7) . ?
C22 H22A 0.9500 . ?
C71 C72 1.394(7) . ?
C71 C76 1.394(7) . ?
C76 C75 1.379(7) . ?
C76 H76A 0.9500 . ?
C75 C74 1.397(7) . ?
C75 H75A 0.9500 . ?
C74 C73 1.368(8) . ?
C74 H74A 0.9500 . ?
C73 C72 1.389(7) . ?
C73 H73A 0.9500 . ?
C72 H72A 0.9500 . ?
C65 C70 1.388(7) . ?
C65 C66 1.396(7) . ?
C66 C67 1.396(8) . ?
C66 H66A 0.9500 . ?
C67 C68 1.371(9) . ?
C67 H67A 0.9500 . ?
C68 C69 1.360(9) . ?
C68 H68A 0.9500 . ?
C69 C70 1.391(8) . ?
C69 H69A 0.9500 . ?
C70 H70A 0.9500 . ?
C59 C64 1.378(7) . ?
C59 C60 1.387(7) . ?
C60 C61 1.385(7) . ?
C60 H60A 0.9500 . ?
C61 C62 1.357(8) . ?
C61 H61A 0.9500 . ?
C62 C63 1.379(9) . ?
C62 H62A 0.9500 . ?
C63 C64 1.394(8) . ?
C63 H63A 0.9500 . ?
C64 H64A 0.9500 . ?
C77 C78 1.366(7) . ?
C77 H77A 0.9500 . ?
C78 H78A 0.9500 . ?
C79 C80 1.362(7) . ?
C79 H79A 0.9500 . ?
C80 H80A 0.9500 . ?
C1S Cl1 1.716(8) . ?
C1S Cl2 1.765(8) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2S Cl4 1.690(15) . ?
C2S Cl3 1.723(14) . ?
C2S H2S1 0.9900 . ?
C2S H2S2 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Os1 N2 83.51(16) . . ?
N1 Os1 O1 93.11(15) . . ?
N2 Os1 O1 175.90(15) . . ?
N1 Os1 O2 176.70(15) . . ?
N2 Os1 O2 93.62(14) . . ?
O1 Os1 O2 89.82(13) . . ?
N1 Os1 N5 87.86(17) . . ?
N2 Os1 N5 92.60(17) . . ?
O1 Os1 N5 89.58(16) . . ?
O2 Os1 N5 90.65(15) . . ?
N1 Os1 N7 90.71(17) . . ?
N2 Os1 N7 88.40(16) . . ?
O1 Os1 N7 89.32(15) . . ?
O2 Os1 N7 90.84(14) . . ?
N5 Os1 N7 178.15(17) . . ?
N3 Os2 N4 83.19(18) . . ?
N3 Os2 O4 175.90(15) . . ?
N4 Os2 O4 93.45(16) . . ?
N3 Os2 O3 93.88(15) . . ?
N4 Os2 O3 177.05(16) . . ?
O4 Os2 O3 89.50(13) . . ?
N3 Os2 N6 91.66(16) . . ?
N4 Os2 N6 88.47(17) . . ?
O4 Os2 N6 90.59(15) . . ?
O3 Os2 N6 91.27(14) . . ?
N3 Os2 N8 89.76(16) . . ?
N4 Os2 N8 90.19(17) . . ?
O4 Os2 N8 87.91(15) . . ?
O3 Os2 N8 90.16(15) . . ?
N6 Os2 N8 177.92(16) . . ?
N5 P1 C53 113.9(2) . . ?
N5 P1 C47 106.9(3) . . ?
C53 P1 C47 106.8(3) . . ?
N5 P1 C41 115.2(2) . . ?
C53 P1 C41 106.2(2) . . ?
C47 P1 C41 107.3(3) . . ?
N6 P2 C65 109.0(2) . . ?
N6 P2 C59 114.1(2) . . ?
C65 P2 C59 105.6(2) . . ?
N6 P2 C71 114.8(2) . . ?
C65 P2 C71 106.2(2) . . ?
C59 P2 C71 106.5(2) . . ?
F6 P3 F5 89.5(3) . . ?
F6 P3 F1 179.1(3) . . ?
F5 P3 F1 90.9(4) . . ?
F6 P3 F4 89.6(3) . . ?
F5 P3 F4 91.6(3) . . ?
F1 P3 F4 91.1(3) . . ?
F6 P3 F2 91.2(3) . . ?
F5 P3 F2 91.0(3) . . ?
F1 P3 F2 88.0(3) . . ?
F4 P3 F2 177.2(3) . . ?
F6 P3 F3 90.8(3) . . ?
F5 P3 F3 179.4(4) . . ?
F1 P3 F3 88.8(4) . . ?
F4 P3 F3 87.9(3) . . ?
F2 P3 F3 89.4(3) . . ?
F7 P4 F10 91.5(3) . . ?
F7 P4 F8 93.0(4) . . ?
F10 P4 F8 175.4(4) . . ?
F7 P4 F11 91.7(3) . . ?
F10 P4 F11 90.4(2) . . ?
F8 P4 F11 90.5(2) . . ?
F7 P4 F12 178.6(3) . . ?
F10 P4 F12 87.5(3) . . ?
F8 P4 F12 88.0(4) . . ?
F11 P4 F12 89.3(3) . . ?
F7 P4 F9 88.3(2) . . ?
F10 P4 F9 90.3(2) . . ?
F8 P4 F9 88.8(2) . . ?
F11 P4 F9 179.3(2) . . ?
F12 P4 F9 90.8(3) . . ?
C20 O2 Os1 124.5(3) . . ?
C1 O1 Os1 123.1(3) . . ?
C40 O4 Os2 123.4(3) . . ?
C21 O3 Os2 124.2(3) . . ?
C14 N2 C13 122.1(4) . . ?
C14 N2 Os1 125.3(3) . . ?
C13 N2 Os1 112.5(3) . . ?
C7 N1 C8 122.2(4) . . ?
C7 N1 Os1 125.2(4) . . ?
C8 N1 Os1 112.2(3) . . ?
P1 N5 Os1 132.0(3) . . ?
P1 N5 H5N 114.0 . . ?
Os1 N5 H5N 114.0 . . ?
C80 N7 C77 115.6(4) . . ?
C80 N7 Os1 122.2(3) . . ?
C77 N7 Os1 121.9(3) . . ?
C34 N4 C33A 121.6(5) . . ?
C34 N4 C33B 121.5(7) . . ?
C33A N4 C33B 24.5(6) . . ?
C34 N4 Os2 124.9(4) . . ?
C33A N4 Os2 112.7(4) . . ?
C33B N4 Os2 111.3(6) . . ?
C27 N3 C28B 119.4(7) . . ?
C27 N3 C28A 122.4(5) . . ?
C28B N3 C28A 22.3(6) . . ?
C27 N3 Os2 124.9(3) . . ?
C28B N3 Os2 113.8(7) . . ?
C28A N3 Os2 112.1(5) . . ?
P2 N6 Os2 131.1(2) . . ?
P2 N6 H6N 114.5 . . ?
Os2 N6 H6N 114.5 . . ?
C78 N8 C79 116.2(4) . . ?
C78 N8 Os2 120.6(3) . . ?
C79 N8 Os2 123.0(3) . . ?
O2 C20 C19 117.3(4) . . ?
O2 C20 C15 124.6(4) . . ?
C19 C20 C15 118.1(4) . . ?
C18 C19 C20 122.2(5) . . ?
C18 C19 H19A 118.9 . . ?
C20 C19 H19A 118.9 . . ?
C19 C18 C17 120.4(5) . . ?
C19 C18 H18A 119.8 . . ?
C17 C18 H18A 119.8 . . ?
C16 C17 C18 119.2(5) . . ?
C16 C17 H17A 120.4 . . ?
C18 C17 H17A 120.4 . . ?
C17 C16 C15 122.5(6) . . ?
C17 C16 H16A 118.8 . . ?
C15 C16 H16A 118.8 . . ?
C16 C15 C20 117.6(5) . . ?
C16 C15 C14 116.2(5) . . ?
C20 C15 C14 126.1(4) . . ?
N2 C14 C15 125.8(4) . . ?
N2 C14 H14A 117.1 . . ?
C15 C14 H14A 117.1 . . ?
C8 C13 C12 114.7(5) . . ?
C8 C13 N2 112.0(5) . . ?
C12 C13 N2 117.8(5) . . ?
C8 C13 H13A 103.4 . . ?
C12 C13 H13A 103.4 . . ?
N2 C13 H13A 103.4 . . ?
C13 C12 C11 112.3(6) . . ?
C13 C12 H12A 109.1 . . ?
C11 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
C10 C11 C12 117.2(6) . . ?
C10 C11 H11A 108.0 . . ?
C12 C11 H11A 108.0 . . ?
C10 C11 H11B 108.0 . . ?
C12 C11 H11B 108.0 . . ?
H11A C11 H11B 107.2 . . ?
C11 C10 C9 116.8(6) . . ?
C11 C10 H10A 108.1 . . ?
C9 C10 H10A 108.1 . . ?
C11 C10 H10B 108.1 . . ?
C9 C10 H10B 108.1 . . ?
H10A C10 H10B 107.3 . . ?
C8 C9 C10 110.4(6) . . ?
C8 C9 H9A 109.6 . . ?
C10 C9 H9A 109.6 . . ?
C8 C9 H9B 109.6 . . ?
C10 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C13 C8 N1 110.3(5) . . ?
C13 C8 C9 114.9(6) . . ?
N1 C8 C9 117.8(5) . . ?
C13 C8 H8A 104.0 . . ?
N1 C8 H8A 104.0 . . ?
C9 C8 H8A 104.0 . . ?
N1 C7 C6 124.9(5) . . ?
N1 C7 H7A 117.5 . . ?
C6 C7 H7A 117.5 . . ?
C1 C6 C5 117.9(5) . . ?
C1 C6 C7 125.8(5) . . ?
C5 C6 C7 116.2(5) . . ?
C4 C5 C6 122.1(6) . . ?
C4 C5 H5A 118.9 . . ?
C6 C5 H5A 118.9 . . ?
C5 C4 C3 119.0(6) . . ?
C5 C4 H4A 120.5 . . ?
C3 C4 H4A 120.5 . . ?
C2 C3 C4 121.2(6) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?
C3 C2 C1 121.5(5) . . ?
C3 C2 H2A 119.2 . . ?
C1 C2 H2A 119.2 . . ?
O1 C1 C2 116.6(5) . . ?
O1 C1 C6 125.0(5) . . ?
C2 C1 C6 118.3(5) . . ?
C42 C41 C46 119.1(5) . . ?
C42 C41 P1 121.1(4) . . ?
C46 C41 P1 119.7(4) . . ?
C41 C42 C43 120.6(5) . . ?
C41 C42 H42A 119.7 . . ?
C43 C42 H42A 119.7 . . ?
C44 C43 C42 120.0(5) . . ?
C44 C43 H43A 120.0 . . ?
C42 C43 H43A 120.0 . . ?
C45 C44 C43 119.9(5) . . ?
C45 C44 H44A 120.0 . . ?
C43 C44 H44A 120.0 . . ?
C44 C45 C46 120.9(5) . . ?
C44 C45 H45A 119.5 . . ?
C46 C45 H45A 119.5 . . ?
C45 C46 C41 119.4(5) . . ?
C45 C46 H46A 120.3 . . ?
C41 C46 H46A 120.3 . . ?
C48 C47 C52 120.0(6) . . ?
C48 C47 P1 119.8(5) . . ?
C52 C47 P1 120.2(5) . . ?
C47 C52 C51 118.8(7) . . ?
C47 C52 H52A 120.6 . . ?
C51 C52 H52A 120.6 . . ?
C50 C51 C52 120.4(7) . . ?
C50 C51 H51A 119.8 . . ?
C52 C51 H51A 119.8 . . ?
C49 C50 C51 121.1(7) . . ?
C49 C50 H50A 119.5 . . ?
C51 C50 H50A 119.5 . . ?
C50 C49 C48 119.2(8) . . ?
C50 C49 H49A 120.4 . . ?
C48 C49 H49A 120.4 . . ?
C47 C48 C49 120.6(7) . . ?
C47 C48 H48A 119.7 . . ?
C49 C48 H48A 119.7 . . ?
C54 C53 C58 120.2(6) . . ?
C54 C53 P1 117.4(4) . . ?
C58 C53 P1 122.3(4) . . ?
C55 C54 C53 119.4(6) . . ?
C55 C54 H54A 120.3 . . ?
C53 C54 H54A 120.3 . . ?
C54 C55 C56 120.3(6) . . ?
C54 C55 H55A 119.8 . . ?
C56 C55 H55A 119.8 . . ?
C57 C56 C55 119.9(6) . . ?
C57 C56 H56A 120.0 . . ?
C55 C56 H56A 120.0 . . ?
C56 C57 C58 120.6(6) . . ?
C56 C57 H57A 119.7 . . ?
C58 C57 H57A 119.7 . . ?
C57 C58 C53 119.5(6) . . ?
C57 C58 H58A 120.3 . . ?
C53 C58 H58A 120.3 . . ?
O4 C40 C39 116.6(5) . . ?
O4 C40 C35 125.1(5) . . ?
C39 C40 C35 118.3(5) . . ?
C38 C39 C40 121.4(6) . . ?
C38 C39 H39A 119.3 . . ?
C40 C39 H39A 119.3 . . ?
C39 C38 C37 120.4(6) . . ?
C39 C38 H38A 119.8 . . ?
C37 C38 H38A 119.8 . . ?
C36 C37 C38 119.1(6) . . ?
C36 C37 H37A 120.5 . . ?
C38 C37 H37A 120.5 . . ?
C37 C36 C35 123.3(7) . . ?
C37 C36 H36A 118.3 . . ?
C35 C36 H36A 118.3 . . ?
C36 C35 C34 116.9(5) . . ?
C36 C35 C40 117.5(6) . . ?
C34 C35 C40 125.5(5) . . ?
N4 C34 C35 125.5(5) . . ?
N4 C34 H34A 117.2 . . ?
C35 C34 H34A 117.2 . . ?
N3 C28A C29A 115.4(9) . . ?
N3 C28A C33A 109.6(8) . . ?
C29A C28A C33A 109.3(11) . . ?
N3 C28A H28A 107.4 . . ?
C29A C28A H28A 107.4 . . ?
C33A C28A H28A 107.4 . . ?
C28A C29A C30A 108.3(13) . . ?
C28A C29A H29A 110.0 . . ?
C30A C29A H29A 110.0 . . ?
C28A C29A H29B 110.0 . . ?
C30A C29A H29B 110.0 . . ?
H29A C29A H29B 108.4 . . ?
C31A C30A C29A 111.5(13) . . ?
C31A C30A H30A 109.3 . . ?
C29A C30A H30A 109.3 . . ?
C31A C30A H30B 109.3 . . ?
C29A C30A H30B 109.3 . . ?
H30A C30A H30B 108.0 . . ?
C30A C31A C32A 112.2(13) . . ?
C30A C31A H31A 109.2 . . ?
C32A C31A H31A 109.2 . . ?
C30A C31A H31B 109.2 . . ?
C32A C31A H31B 109.2 . . ?
H31A C31A H31B 107.9 . . ?
C33A C32A C31A 103.8(10) . . ?
C33A C32A H32A 111.0 . . ?
C31A C32A H32A 111.0 . . ?
C33A C32A H32B 111.0 . . ?
C31A C32A H32B 111.0 . . ?
H32A C32A H32B 109.0 . . ?
N4 C33A C28A 106.0(7) . . ?
N4 C33A C32A 114.5(9) . . ?
C28A C33A C32A 111.3(10) . . ?
N4 C33A H33A 108.3 . . ?
C28A C33A H33A 108.3 . . ?
C32A C33A H33A 108.3 . . ?
N3 C28B C29B 119.5(15) . . ?
N3 C28B C33B 105.1(13) . . ?
C29B C28B C33B 110.9(17) . . ?
N3 C28B H28B 106.9 . . ?
C29B C28B H28B 106.9 . . ?
C33B C28B H28B 106.9 . . ?
C28B C29B C30B 111(2) . . ?
C28B C29B H29C 109.4 . . ?
C30B C29B H29C 109.4 . . ?
C28B C29B H29D 109.4 . . ?
C30B C29B H29D 109.4 . . ?
H29C C29B H29D 108.0 . . ?
C29B C30B C31B 113(2) . . ?
C29B C30B H30C 109.0 . . ?
C31B C30B H30C 109.0 . . ?
C29B C30B H30D 109.0 . . ?
C31B C30B H30D 109.0 . . ?
H30C C30B H30D 107.8 . . ?
C32B C31B C30B 109.9(19) . . ?
C32B C31B H31C 109.7 . . ?
C30B C31B H31C 109.7 . . ?
C32B C31B H31D 109.7 . . ?
C30B C31B H31D 109.7 . . ?
H31C C31B H31D 108.2 . . ?
C33B C32B C31B 113(2) . . ?
C33B C32B H32C 108.9 . . ?
C31B C32B H32C 108.9 . . ?
C33B C32B H32D 108.9 . . ?
C31B C32B H32D 108.9 . . ?
H32C C32B H32D 107.7 . . ?
N4 C33B C32B 114.7(13) . . ?
N4 C33B C28B 110.1(12) . . ?
C32B C33B C28B 106.8(16) . . ?
N4 C33B H33B 108.4 . . ?
C32B C33B H33B 108.4 . . ?
C28B C33B H33B 108.4 . . ?
N3 C27 C26 125.7(5) . . ?
N3 C27 H27A 117.1 . . ?
C26 C27 H27A 117.1 . . ?
C25 C26 C21 118.2(5) . . ?
C25 C26 C27 115.5(5) . . ?
C21 C26 C27 126.3(5) . . ?
C24 C25 C26 122.1(5) . . ?
C24 C25 H25A 118.9 . . ?
C26 C25 H25A 118.9 . . ?
C25 C24 C23 119.1(5) . . ?
C25 C24 H24A 120.4 . . ?
C23 C24 H24A 120.4 . . ?
C22 C23 C24 120.3(5) . . ?
C22 C23 H23A 119.9 . . ?
C24 C23 H23A 119.9 . . ?
C23 C22 C21 121.7(5) . . ?
C23 C22 H22A 119.2 . . ?
C21 C22 H22A 119.2 . . ?
O3 C21 C22 116.5(4) . . ?
O3 C21 C26 124.9(4) . . ?
C22 C21 C26 118.5(5) . . ?
C72 C71 C76 119.2(4) . . ?
C72 C71 P2 119.4(4) . . ?
C76 C71 P2 121.3(4) . . ?
C75 C76 C71 120.0(5) . . ?
C75 C76 H76A 120.0 . . ?
C71 C76 H76A 120.0 . . ?
C76 C75 C74 120.5(5) . . ?
C76 C75 H75A 119.7 . . ?
C74 C75 H75A 119.7 . . ?
C73 C74 C75 119.5(5) . . ?
C73 C74 H74A 120.3 . . ?
C75 C74 H74A 120.3 . . ?
C74 C73 C72 120.7(5) . . ?
C74 C73 H73A 119.7 . . ?
C72 C73 H73A 119.7 . . ?
C73 C72 C71 120.1(5) . . ?
C73 C72 H72A 119.9 . . ?
C71 C72 H72A 119.9 . . ?
C70 C65 C66 119.1(5) . . ?
C70 C65 P2 119.5(4) . . ?
C66 C65 P2 121.0(4) . . ?
C65 C66 C67 119.5(5) . . ?
C65 C66 H66A 120.2 . . ?
C67 C66 H66A 120.2 . . ?
C68 C67 C66 120.2(5) . . ?
C68 C67 H67A 119.9 . . ?
C66 C67 H67A 119.9 . . ?
C69 C68 C67 120.8(5) . . ?
C69 C68 H68A 119.6 . . ?
C67 C68 H68A 119.6 . . ?
C68 C69 C70 120.0(6) . . ?
C68 C69 H69A 120.0 . . ?
C70 C69 H69A 120.0 . . ?
C65 C70 C69 120.3(5) . . ?
C65 C70 H70A 119.8 . . ?
C69 C70 H70A 119.8 . . ?
C64 C59 C60 119.7(5) . . ?
C64 C59 P2 117.3(4) . . ?
C60 C59 P2 122.9(4) . . ?
C61 C60 C59 120.2(5) . . ?
C61 C60 H60A 119.9 . . ?
C59 C60 H60A 119.9 . . ?
C62 C61 C60 120.3(5) . . ?
C62 C61 H61A 119.9 . . ?
C60 C61 H61A 119.9 . . ?
C61 C62 C63 119.9(5) . . ?
C61 C62 H62A 120.0 . . ?
C63 C62 H62A 120.0 . . ?
C62 C63 C64 120.7(6) . . ?
C62 C63 H63A 119.7 . . ?
C64 C63 H63A 119.7 . . ?
C59 C64 C63 119.1(5) . . ?
C59 C64 H64A 120.4 . . ?
C63 C64 H64A 120.4 . . ?
N7 C77 C78 122.1(4) . . ?
N7 C77 H77A 118.9 . . ?
C78 C77 H77A 118.9 . . ?
N8 C78 C77 121.8(5) . . ?
N8 C78 H78A 119.1 . . ?
C77 C78 H78A 119.1 . . ?
N8 C79 C80 122.3(4) . . ?
N8 C79 H79A 118.9 . . ?
C80 C79 H79A 118.9 . . ?
N7 C80 C79 121.7(5) . . ?
N7 C80 H80A 119.1 . . ?
C79 C80 H80A 119.1 . . ?
Cl1 C1S Cl2 113.1(4) . . ?
Cl1 C1S H1SA 109.0 . . ?
Cl2 C1S H1SA 109.0 . . ?
Cl1 C1S H1SB 109.0 . . ?
Cl2 C1S H1SB 109.0 . . ?
H1SA C1S H1SB 107.8 . . ?
Cl4 C2S Cl3 114.8(8) . . ?
Cl4 C2S H2S1 108.6 . . ?
Cl3 C2S H2S1 108.6 . . ?
Cl4 C2S H2S2 108.6 . . ?
Cl3 C2S H2S2 108.6 . . ?
H2S1 C2S H2S2 107.5 . . ?

_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        67.00
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         1.270
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.101

data_5
_database_code_depnum_ccdc_archive 'CCDC 793801'
#TrackingRef '- Os(salen)binuclear.Dalton(CIF).cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C73 H75.50 F12 N8.50 O6 Os2 P4'
_chemical_formula_weight         1900.20

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 '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'
H H 0.0000 0.0000 '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                   19.3433(4)
_cell_length_b                   16.2405(3)
_cell_length_c                   25.7370(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.477(2)
_cell_angle_gamma                90.00
_cell_volume                     7792.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    26377
_cell_measurement_theta_min      3.4130
_cell_measurement_theta_max      28.0521

_exptl_crystal_description       needle
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3764
_exptl_absorpt_coefficient_mu    3.424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlis RED, Oxford Diffraction Ltd'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.1270
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            85318
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0712
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.41
_diffrn_reflns_theta_max         25.00
_reflns_number_total             13665
_reflns_number_gt                8641
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep-3
_computing_publication_material  Wingx

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         13665
_refine_ls_number_parameters     965
_refine_ls_number_restraints     157
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0696
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      1.001
_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
Os1 Os 0.107572(12) 1.014475(12) 0.354846(9) 0.03923(7) Uani 1 1 d . . .
Os2 Os 0.328042(13) 0.594631(13) 0.466179(10) 0.04772(8) Uani 1 1 d . A .
P1 P 0.27434(8) 0.95221(8) 0.40802(6) 0.0377(4) Uani 1 1 d . . .
P2 P 0.21649(8) 0.67622(8) 0.35635(6) 0.0390(4) Uani 1 1 d . A .
P3 P 0.20034(13) 0.24061(12) 0.08941(9) 0.0817(6) Uani 1 1 d D . .
P4 P 0.4309(2) 0.4941(3) 0.26996(14) 0.1468(12) Uani 1 1 d D . .
F1 F 0.1794(3) 0.2180(3) 0.1424(2) 0.175(3) Uani 1 1 d D . .
F2 F 0.2737(3) 0.2674(4) 0.1249(2) 0.181(3) Uani 1 1 d D . .
F3 F 0.1737(4) 0.3275(3) 0.0962(2) 0.200(3) Uani 1 1 d D . .
F4 F 0.1253(4) 0.2205(6) 0.0532(3) 0.255(4) Uani 1 1 d D . .
F5 F 0.2261(6) 0.1566(3) 0.0851(3) 0.297(6) Uani 1 1 d D . .
F6 F 0.2183(3) 0.2694(4) 0.0373(2) 0.168(2) Uani 1 1 d D . .
F7 F 0.3959(4) 0.4143(5) 0.2867(3) 0.230(4) Uani 1 1 d D . .
F8 F 0.4948(4) 0.4810(5) 0.3208(4) 0.238(4) Uani 1 1 d D . .
F9 F 0.3987(5) 0.5478(7) 0.3053(3) 0.335(7) Uani 1 1 d D . .
F10 F 0.3584(5) 0.5129(5) 0.2254(3) 0.266(5) Uani 1 1 d D . .
F11 F 0.4510(6) 0.4379(5) 0.2297(4) 0.336(7) Uani 1 1 d D . .
F12 F 0.4702(7) 0.5611(5) 0.2490(4) 0.316(6) Uani 1 1 d D . .
O1 O 0.11294(19) 0.92754(19) 0.41095(14) 0.0436(9) Uani 1 1 d . . .
O2 O 0.11470(19) 0.92821(19) 0.30089(14) 0.0460(10) Uani 1 1 d . . .
O3 O 0.3792(2) 0.7011(2) 0.46441(16) 0.0552(11) Uani 1 1 d . . .
O4 O 0.2502(2) 0.6560(2) 0.48809(15) 0.0523(10) Uani 1 1 d . . .
O5 O 0.0047(2) 1.0124(2) 0.33249(15) 0.0541(10) Uani 1 1 d . . .
O6 O 0.3782(2) 0.5762(2) 0.53953(16) 0.0724(13) Uani 1 1 d . . .
N1 N 0.1033(2) 1.1071(2) 0.40514(18) 0.0410(11) Uani 1 1 d . . .
N2 N 0.1062(2) 1.1065(2) 0.30305(18) 0.0452(12) Uani 1 1 d . . .
N3 N 0.4001(3) 0.5285(3) 0.4427(2) 0.0540(13) Uani 1 1 d D . .
N4 N 0.2798(3) 0.4853(3) 0.46654(19) 0.0515(13) Uani 1 1 d D . .
N5 N 0.2172(2) 1.0185(2) 0.37640(17) 0.0427(11) Uani 1 1 d . . .
H5 H 0.2354 1.0626 0.3670 0.051 Uiso 1 1 calc R . .
N6 N 0.2749(2) 0.6109(2) 0.38618(16) 0.0437(12) Uani 1 1 d . . .
H6 H 0.2864 0.5758 0.3649 0.052 Uiso 1 1 calc R A .
C1 C 0.1014(3) 0.9420(3) 0.4586(2) 0.0405(13) Uani 1 1 d . . .
C2 C 0.0953(3) 0.8732(3) 0.4895(2) 0.0529(16) Uani 1 1 d . . .
H2 H 0.0982 0.8209 0.4754 0.063 Uiso 1 1 calc R . .
C3 C 0.0851(3) 0.8804(4) 0.5399(2) 0.0595(17) Uani 1 1 d . . .
H3 H 0.0810 0.8334 0.5595 0.071 Uiso 1 1 calc R . .
C4 C 0.0808(3) 0.9576(4) 0.5619(2) 0.0587(17) Uani 1 1 d . . .
H4 H 0.0733 0.9628 0.5959 0.070 Uiso 1 1 calc R . .
C5 C 0.0877(3) 1.0247(3) 0.5331(2) 0.0494(15) Uani 1 1 d . . .
H5A H 0.0862 1.0762 0.5487 0.059 Uiso 1 1 calc R . .
C6 C 0.0971(3) 1.0214(3) 0.4813(2) 0.0401(13) Uani 1 1 d . . .
C7 C 0.1002(3) 1.0968(3) 0.4544(2) 0.0457(14) Uani 1 1 d . . .
H7 H 0.1000 1.1445 0.4744 0.055 Uiso 1 1 calc R . .
C8 C 0.1088(4) 1.1889(3) 0.3813(3) 0.0595(18) Uani 1 1 d . . .
H8 H 0.1601 1.2005 0.3879 0.071 Uiso 1 1 calc R . .
C9 C 0.0772(4) 1.2604(3) 0.4057(3) 0.0645(19) Uani 1 1 d . . .
H9A H 0.0275 1.2486 0.4041 0.077 Uiso 1 1 calc R . .
H9B H 0.1033 1.2668 0.4433 0.077 Uiso 1 1 calc R . .
C10 C 0.0814(5) 1.3396(4) 0.3755(3) 0.094(3) Uani 1 1 d . . .
H10A H 0.0543 1.3818 0.3882 0.113 Uiso 1 1 calc R . .
H10B H 0.1310 1.3574 0.3841 0.113 Uiso 1 1 calc R . .
C11 C 0.0539(4) 1.3326(4) 0.3164(3) 0.090(2) Uani 1 1 d . . .
H11A H 0.0643 1.3834 0.3001 0.108 Uiso 1 1 calc R . .
H11B H 0.0021 1.3265 0.3073 0.108 Uiso 1 1 calc R . .
C12 C 0.0850(4) 1.2614(3) 0.2923(2) 0.0646(18) Uani 1 1 d . . .
H12A H 0.0597 1.2558 0.2545 0.078 Uiso 1 1 calc R . .
H12B H 0.1351 1.2724 0.2947 0.078 Uiso 1 1 calc R . .
C13 C 0.0790(3) 1.1829(3) 0.3212(2) 0.0556(17) Uani 1 1 d . . .
H13 H 0.0274 1.1739 0.3153 0.067 Uiso 1 1 calc R . .
C14 C 0.1233(3) 1.0991(3) 0.2592(2) 0.0529(16) Uani 1 1 d . . .
H14 H 0.1215 1.1464 0.2386 0.064 Uiso 1 1 calc R . .
C15 C 0.1450(3) 1.0245(4) 0.2385(2) 0.0555(16) Uani 1 1 d . . .
C16 C 0.1726(5) 1.0314(4) 0.1941(3) 0.095(3) Uani 1 1 d . . .
H16 H 0.1777 1.0837 0.1809 0.114 Uiso 1 1 calc R . .
C17 C 0.1923(6) 0.9656(6) 0.1691(3) 0.130(4) Uani 1 1 d U . .
H17 H 0.2107 0.9724 0.1395 0.156 Uiso 1 1 calc R . .
C18 C 0.1844(6) 0.8880(5) 0.1888(3) 0.118(3) Uani 1 1 d . . .
H18 H 0.1979 0.8420 0.1723 0.142 Uiso 1 1 calc R . .
C19 C 0.1572(4) 0.8781(4) 0.2319(3) 0.081(2) Uani 1 1 d . . .
H19 H 0.1518 0.8250 0.2439 0.097 Uiso 1 1 calc R . .
C20 C 0.1371(3) 0.9443(3) 0.2587(2) 0.0517(16) Uani 1 1 d . . .
C21 C 0.4349(3) 0.7092(4) 0.4457(2) 0.0528(16) Uani 1 1 d . A .
C22 C 0.4607(4) 0.7896(4) 0.4432(3) 0.072(2) Uani 1 1 d . . .
H22 H 0.4376 0.8336 0.4545 0.087 Uiso 1 1 calc R . .
C23 C 0.5193(5) 0.8041(5) 0.4244(3) 0.094(3) Uani 1 1 d . . .
H23 H 0.5345 0.8581 0.4227 0.112 Uiso 1 1 calc R . .
C24 C 0.5567(5) 0.7415(6) 0.4080(3) 0.101(3) Uani 1 1 d . . .
H24 H 0.5974 0.7520 0.3964 0.121 Uiso 1 1 calc R . .
C25 C 0.5313(4) 0.6632(5) 0.4094(3) 0.082(2) Uani 1 1 d . A .
H25 H 0.5551 0.6206 0.3973 0.099 Uiso 1 1 calc R . .
C26 C 0.4718(3) 0.6434(4) 0.4279(2) 0.0558(16) Uani 1 1 d . . .
C27 C 0.4534(4) 0.5577(4) 0.4285(2) 0.0561(17) Uani 1 1 d . A .
H27 H 0.4830 0.5202 0.4176 0.067 Uiso 1 1 calc R . .
C28A C 0.3870(5) 0.4360(6) 0.4556(5) 0.037(3) Uiso 0.50 1 d PD A 1
H28A H 0.4045 0.4262 0.4945 0.044 Uiso 0.50 1 calc PR A 1
C29A C 0.4226(7) 0.3756(7) 0.4252(5) 0.041(4) Uiso 0.50 1 d PD A 1
H29A H 0.4070 0.3881 0.3870 0.050 Uiso 0.50 1 calc PR A 1
H29B H 0.4742 0.3834 0.4370 0.050 Uiso 0.50 1 calc PR A 1
C30A C 0.4060(7) 0.2877(7) 0.4335(6) 0.052(3) Uiso 0.50 1 d PD A 1
H30A H 0.4270 0.2726 0.4708 0.062 Uiso 0.50 1 calc PR A 1
H30B H 0.4269 0.2529 0.4111 0.062 Uiso 0.50 1 calc PR A 1
C31A C 0.3255(7) 0.2740(8) 0.4192(6) 0.072(5) Uiso 0.50 1 d PD A 1
H31A H 0.3153 0.2169 0.4253 0.086 Uiso 0.50 1 calc PR A 1
H31B H 0.3045 0.2866 0.3814 0.086 Uiso 0.50 1 calc PR A 1
C32A C 0.2925(11) 0.3309(8) 0.4549(8) 0.063(6) Uiso 0.50 1 d PD A 1
H32A H 0.3161 0.3227 0.4928 0.075 Uiso 0.50 1 calc PR A 1
H32B H 0.2416 0.3199 0.4488 0.075 Uiso 0.50 1 calc PR A 1
C33A C 0.3052(6) 0.4208(6) 0.4369(6) 0.049(4) Uiso 0.50 1 d PD A 1
H33A H 0.2865 0.4280 0.3979 0.059 Uiso 0.50 1 calc PR A 1
C28B C 0.3824(7) 0.4449(8) 0.4270(7) 0.067(4) Uiso 0.50 1 d PD A 2
H28B H 0.3497 0.4502 0.3908 0.081 Uiso 0.50 1 calc PR A 2
C29B C 0.4409(8) 0.3886(7) 0.4183(7) 0.061(5) Uiso 0.50 1 d PD A 2
H29C H 0.4813 0.3880 0.4502 0.073 Uiso 0.50 1 calc PR A 2
H29D H 0.4576 0.4079 0.3881 0.073 Uiso 0.50 1 calc PR A 2
C30B C 0.4091(8) 0.3011(8) 0.4067(7) 0.087(5) Uiso 0.50 1 d PD A 2
H30C H 0.3826 0.2987 0.3690 0.104 Uiso 0.50 1 calc PR A 2
H30D H 0.4487 0.2626 0.4118 0.104 Uiso 0.50 1 calc PR A 2
C31B C 0.3599(10) 0.2709(9) 0.4399(7) 0.079(5) Uiso 0.50 1 d PD A 2
H31C H 0.3885 0.2578 0.4760 0.095 Uiso 0.50 1 calc PR A 2
H31D H 0.3363 0.2207 0.4239 0.095 Uiso 0.50 1 calc PR A 2
C32B C 0.3026(11) 0.3346(9) 0.4434(9) 0.081(8) Uiso 0.50 1 d PD A 2
H32C H 0.2679 0.3390 0.4085 0.097 Uiso 0.50 1 calc PR A 2
H32D H 0.2774 0.3154 0.4691 0.097 Uiso 0.50 1 calc PR A 2
C33B C 0.3339(9) 0.4196(7) 0.4607(6) 0.062(4) Uiso 0.50 1 d PD A 2
H33B H 0.3655 0.4120 0.4971 0.074 Uiso 0.50 1 calc PR A 2
C34 C 0.2243(4) 0.4729(4) 0.4828(2) 0.0619(18) Uani 1 1 d . A .
H34 H 0.2084 0.4188 0.4826 0.074 Uiso 1 1 calc R . .
C35 C 0.1838(4) 0.5348(4) 0.5016(3) 0.0616(18) Uani 1 1 d . . .
C36 C 0.1237(4) 0.5067(5) 0.5181(3) 0.088(2) Uani 1 1 d . A .
H36 H 0.1138 0.4506 0.5162 0.106 Uiso 1 1 calc R . .
C37 C 0.0804(5) 0.5569(6) 0.5362(4) 0.108(3) Uani 1 1 d . . .
H37 H 0.0400 0.5369 0.5451 0.130 Uiso 1 1 calc R A .
C38 C 0.0981(5) 0.6401(6) 0.5414(4) 0.107(3) Uani 1 1 d . A .
H38 H 0.0705 0.6755 0.5559 0.129 Uiso 1 1 calc R . .
C39 C 0.1548(4) 0.6713(4) 0.5257(3) 0.080(2) Uani 1 1 d . . .
H39 H 0.1645 0.7274 0.5289 0.096 Uiso 1 1 calc R A .
C40 C 0.1991(3) 0.6191(4) 0.5046(2) 0.0548(16) Uani 1 1 d . A .
C41 C 0.3577(3) 0.9745(3) 0.3947(2) 0.0456(14) Uani 1 1 d . . .
C42 C 0.4105(4) 1.0195(4) 0.4307(3) 0.0663(18) Uani 1 1 d . . .
H42 H 0.4051 1.0321 0.4647 0.080 Uiso 1 1 calc R . .
C43 C 0.4706(4) 1.0456(5) 0.4164(4) 0.093(3) Uani 1 1 d . . .
H43 H 0.5049 1.0774 0.4402 0.112 Uiso 1 1 calc R . .
C44 C 0.4799(5) 1.0255(5) 0.3684(4) 0.096(3) Uani 1 1 d . . .
H44 H 0.5209 1.0427 0.3591 0.115 Uiso 1 1 calc R . .
C45 C 0.4289(5) 0.9792(5) 0.3325(4) 0.095(3) Uani 1 1 d . . .
H45 H 0.4361 0.9643 0.2994 0.114 Uiso 1 1 calc R . .
C46 C 0.3683(4) 0.9554(4) 0.3454(3) 0.0700(19) Uani 1 1 d . . .
H46 H 0.3335 0.9257 0.3205 0.084 Uiso 1 1 calc R . .
C47 C 0.2853(3) 0.9487(3) 0.4785(2) 0.0391(13) Uani 1 1 d . . .
C48 C 0.3029(3) 0.8772(3) 0.5082(2) 0.0510(15) Uani 1 1 d . . .
H48 H 0.3049 0.8276 0.4906 0.061 Uiso 1 1 calc R . .
C49 C 0.3174(4) 0.8785(4) 0.5635(3) 0.0673(19) Uani 1 1 d . . .
H49 H 0.3294 0.8300 0.5830 0.081 Uiso 1 1 calc R . .
C50 C 0.3143(4) 0.9512(5) 0.5900(3) 0.0704(19) Uani 1 1 d . . .
H50 H 0.3250 0.9521 0.6274 0.084 Uiso 1 1 calc R . .
C51 C 0.2952(3) 1.0224(4) 0.5612(3) 0.0680(19) Uani 1 1 d . . .
H51 H 0.2919 1.0714 0.5790 0.082 Uiso 1 1 calc R . .
C52 C 0.2812(3) 1.0215(3) 0.5061(2) 0.0529(16) Uani 1 1 d . . .
H52 H 0.2686 1.0702 0.4869 0.064 Uiso 1 1 calc R . .
C53 C 0.1300(3) 0.6638(3) 0.3666(2) 0.0404(14) Uani 1 1 d . . .
C54 C 0.1035(3) 0.5850(4) 0.3666(3) 0.0600(18) Uani 1 1 d . A .
H54 H 0.1317 0.5403 0.3625 0.072 Uiso 1 1 calc R . .
C55 C 0.0361(4) 0.5718(4) 0.3727(3) 0.076(2) Uani 1 1 d . . .
H55 H 0.0187 0.5184 0.3725 0.091 Uiso 1 1 calc R A .
C56 C -0.0053(4) 0.6368(4) 0.3791(3) 0.074(2) Uani 1 1 d . A .
H56 H -0.0508 0.6279 0.3838 0.089 Uiso 1 1 calc R . .
C57 C 0.0201(4) 0.7146(4) 0.3785(3) 0.0641(18) Uani 1 1 d . . .
H57 H -0.0084 0.7590 0.3825 0.077 Uiso 1 1 calc R A .
C58 C 0.0872(3) 0.7286(3) 0.3722(2) 0.0542(16) Uani 1 1 d . A .
H58 H 0.1038 0.7823 0.3717 0.065 Uiso 1 1 calc R . .
C59 C 0.2089(3) 0.6704(3) 0.2859(2) 0.0417(14) Uani 1 1 d . . .
C60 C 0.2687(4) 0.6827(4) 0.2683(3) 0.072(2) Uani 1 1 d . A .
H60 H 0.3120 0.6963 0.2927 0.086 Uiso 1 1 calc R . .
C61 C 0.2645(4) 0.6748(5) 0.2139(3) 0.090(2) Uani 1 1 d . . .
H61 H 0.3052 0.6834 0.2018 0.109 Uiso 1 1 calc R A .
C62 C 0.2015(4) 0.6548(4) 0.1783(3) 0.078(2) Uani 1 1 d . A .
H62 H 0.1990 0.6496 0.1419 0.094 Uiso 1 1 calc R . .
C63 C 0.1430(4) 0.6424(4) 0.1954(3) 0.0676(19) Uani 1 1 d . . .
H63 H 0.1001 0.6282 0.1707 0.081 Uiso 1 1 calc R A .
C64 C 0.1452(3) 0.6504(3) 0.2489(2) 0.0537(16) Uani 1 1 d . A .
H64 H 0.1038 0.6423 0.2601 0.064 Uiso 1 1 calc R . .
C65 C 0.2527(3) 0.8492(3) 0.3860(2) 0.0386(13) Uani 1 1 d . A .
C66 C 0.2414(3) 0.7785(3) 0.3761(2) 0.0393(14) Uani 1 1 d . . .
C67 C -0.0310(3) 0.9361(4) 0.3247(3) 0.076(2) Uani 1 1 d . . .
H67A H -0.0125 0.9029 0.3006 0.114 Uiso 1 1 calc R . .
H67B H -0.0814 0.9449 0.3095 0.114 Uiso 1 1 calc R . .
H67C H -0.0234 0.9084 0.3587 0.114 Uiso 1 1 calc R . .
C68 C 0.3827(4) 0.6400(4) 0.5784(3) 0.102(3) Uani 1 1 d . . .
H68A H 0.4074 0.6865 0.5688 0.152 Uiso 1 1 calc R . .
H68B H 0.4086 0.6202 0.6134 0.152 Uiso 1 1 calc R . .
H68C H 0.3353 0.6561 0.5792 0.152 Uiso 1 1 calc R . .
N1S N 0.2125(4) 0.4485(4) 0.3060(3) 0.108(2) Uani 1 1 d U . .
N2S N 0.2838(5) 0.1549(6) 0.3125(4) 0.134(3) Uani 1 1 d U . .
N3S N 0.5553(11) 0.2250(11) 0.3265(8) 0.152(7) Uani 0.50 1 d PDU . .
C1S C 0.2346(6) 0.3862(7) 0.2217(4) 0.186(5) Uani 1 1 d U . .
H1S1 H 0.2038 0.3394 0.2108 0.280 Uiso 1 1 calc R . .
H1S2 H 0.2837 0.3692 0.2287 0.280 Uiso 1 1 calc R . .
H1S3 H 0.2243 0.4266 0.1934 0.280 Uiso 1 1 calc R . .
C2S C 0.2222(5) 0.4220(5) 0.2708(4) 0.100(3) Uani 1 1 d U . .
C3S C 0.3646(7) 0.1768(9) 0.2518(5) 0.219(6) Uani 1 1 d U . .
H3S1 H 0.4117 0.1913 0.2734 0.329 Uiso 1 1 calc R . .
H3S2 H 0.3463 0.2203 0.2266 0.329 Uiso 1 1 calc R . .
H3S3 H 0.3673 0.1269 0.2325 0.329 Uiso 1 1 calc R . .
C4S C 0.3175(7) 0.1648(8) 0.2862(5) 0.138(4) Uani 1 1 d U . .
C5S C 0.5325(12) 0.2659(12) 0.2318(9) 0.154(7) Uani 0.50 1 d PDU . .
H5S1 H 0.5439 0.2193 0.2126 0.231 Uiso 0.50 1 calc PR . .
H5S2 H 0.5572 0.3136 0.2239 0.231 Uiso 0.50 1 calc PR . .
H5S3 H 0.4817 0.2755 0.2208 0.231 Uiso 0.50 1 calc PR . .
C6S C 0.5537(13) 0.2503(14) 0.2862(10) 0.139(7) Uani 0.50 1 d PDU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os1 0.04423(15) 0.03439(12) 0.03538(13) 0.00329(10) 0.00423(10) 0.00532(11)
Os2 0.04649(16) 0.04184(14) 0.04682(16) -0.00241(11) -0.00151(12) 0.01219(12)
P1 0.0391(9) 0.0339(8) 0.0376(9) -0.0001(6) 0.0060(7) 0.0021(6)
P2 0.0419(9) 0.0325(8) 0.0380(9) -0.0047(6) 0.0025(7) 0.0061(7)
P3 0.1023(18) 0.0593(13) 0.0800(16) 0.0090(10) 0.0181(14) -0.0149(12)
P4 0.160(3) 0.199(4) 0.093(2) 0.026(2) 0.053(2) 0.006(3)
F1 0.235(7) 0.171(5) 0.128(5) 0.050(4) 0.062(5) -0.058(5)
F2 0.108(5) 0.278(8) 0.144(5) -0.016(5) 0.011(4) -0.037(5)
F3 0.306(9) 0.136(5) 0.158(6) 0.036(4) 0.063(6) 0.104(5)
F4 0.165(7) 0.402(12) 0.163(7) 0.014(7) -0.015(5) -0.153(8)
F5 0.572(16) 0.087(4) 0.168(7) -0.029(4) -0.013(8) 0.115(6)
F6 0.190(6) 0.236(6) 0.096(4) 0.019(4) 0.068(4) 0.007(5)
F7 0.223(8) 0.312(10) 0.163(7) 0.074(7) 0.064(6) -0.036(7)
F8 0.123(6) 0.280(9) 0.277(11) 0.045(8) -0.002(6) 0.015(6)
F9 0.370(13) 0.498(15) 0.103(6) -0.063(7) 0.006(7) 0.296(12)
F10 0.367(13) 0.283(10) 0.111(6) 0.029(6) 0.000(7) 0.102(10)
F11 0.56(2) 0.216(8) 0.378(14) -0.054(9) 0.378(16) -0.038(10)
F12 0.513(19) 0.214(8) 0.276(11) -0.001(8) 0.200(13) -0.143(10)
O1 0.058(3) 0.036(2) 0.037(2) 0.0028(17) 0.014(2) 0.0027(18)
O2 0.057(3) 0.043(2) 0.033(2) -0.0024(18) 0.0050(19) 0.0043(19)
O3 0.040(3) 0.048(2) 0.069(3) -0.011(2) 0.000(2) 0.007(2)
O4 0.055(3) 0.045(2) 0.054(3) 0.0005(19) 0.011(2) 0.013(2)
O5 0.052(3) 0.045(2) 0.063(3) -0.0041(19) 0.010(2) 0.003(2)
O6 0.088(3) 0.065(3) 0.049(3) -0.009(2) -0.008(2) 0.020(2)
N1 0.049(3) 0.033(3) 0.037(3) 0.000(2) 0.004(2) 0.002(2)
N2 0.056(3) 0.044(3) 0.031(3) 0.005(2) 0.004(2) 0.013(2)
N3 0.044(3) 0.050(3) 0.054(3) -0.005(2) -0.012(3) 0.008(3)
N4 0.064(4) 0.034(3) 0.052(3) 0.001(2) 0.007(3) 0.006(3)
N5 0.051(3) 0.031(2) 0.045(3) 0.007(2) 0.010(2) 0.002(2)
N6 0.046(3) 0.045(3) 0.035(3) -0.005(2) 0.002(2) 0.018(2)
C1 0.040(4) 0.043(3) 0.040(4) 0.003(3) 0.013(3) 0.003(3)
C2 0.078(5) 0.036(3) 0.045(4) 0.002(3) 0.018(3) 0.003(3)
C3 0.073(5) 0.064(4) 0.044(4) 0.017(3) 0.020(4) 0.003(3)
C4 0.077(5) 0.065(4) 0.037(4) 0.004(3) 0.020(3) 0.011(3)
C5 0.063(4) 0.044(4) 0.041(4) -0.003(3) 0.013(3) 0.010(3)
C6 0.046(4) 0.036(3) 0.039(3) 0.002(3) 0.011(3) 0.004(3)
C7 0.054(4) 0.040(3) 0.040(4) -0.007(3) 0.005(3) 0.010(3)
C8 0.080(5) 0.030(3) 0.065(5) 0.012(3) 0.013(4) 0.001(3)
C9 0.094(5) 0.034(3) 0.066(5) 0.000(3) 0.022(4) 0.013(3)
C10 0.155(8) 0.042(4) 0.083(6) 0.010(4) 0.025(6) 0.029(4)
C11 0.127(7) 0.052(4) 0.089(6) 0.022(4) 0.026(5) 0.033(4)
C12 0.083(5) 0.047(4) 0.059(4) 0.016(3) 0.010(4) 0.015(3)
C13 0.069(5) 0.043(4) 0.054(4) 0.007(3) 0.016(4) 0.016(3)
C14 0.077(5) 0.033(3) 0.042(4) 0.008(3) 0.003(3) 0.016(3)
C15 0.079(5) 0.051(4) 0.037(4) 0.008(3) 0.017(3) 0.012(3)
C16 0.171(9) 0.062(5) 0.068(5) 0.018(4) 0.057(6) 0.026(5)
C17 0.227(11) 0.101(7) 0.081(6) 0.013(5) 0.076(7) 0.028(7)
C18 0.232(11) 0.064(6) 0.083(6) -0.007(4) 0.085(7) 0.033(6)
C19 0.145(7) 0.054(4) 0.044(4) 0.005(3) 0.026(5) 0.020(4)
C20 0.083(5) 0.039(4) 0.028(4) 0.004(3) 0.005(3) 0.014(3)
C21 0.044(4) 0.061(4) 0.044(4) 0.000(3) -0.005(3) 0.006(4)
C22 0.052(5) 0.069(5) 0.088(6) 0.004(4) 0.005(4) 0.005(4)
C23 0.074(6) 0.084(6) 0.116(7) 0.039(5) 0.013(5) -0.001(5)
C24 0.082(7) 0.119(8) 0.112(7) 0.034(6) 0.042(5) 0.013(6)
C25 0.082(6) 0.093(6) 0.079(6) 0.011(4) 0.033(5) 0.020(5)
C26 0.052(4) 0.070(5) 0.040(4) 0.006(3) 0.003(3) 0.010(4)
C27 0.054(5) 0.054(4) 0.052(4) -0.016(3) -0.001(3) 0.012(3)
C34 0.073(5) 0.049(4) 0.061(5) 0.010(3) 0.014(4) -0.001(4)
C35 0.070(5) 0.052(4) 0.062(5) 0.012(3) 0.017(4) 0.017(4)
C36 0.083(6) 0.071(5) 0.116(7) 0.027(5) 0.038(5) 0.008(5)
C37 0.102(7) 0.083(6) 0.162(9) 0.036(6) 0.076(7) 0.023(5)
C38 0.097(7) 0.094(7) 0.155(9) 0.028(6) 0.076(7) 0.035(5)
C39 0.090(6) 0.063(4) 0.097(6) 0.024(4) 0.042(5) 0.035(4)
C40 0.051(4) 0.062(5) 0.049(4) 0.011(3) 0.009(3) 0.009(3)
C41 0.042(4) 0.042(3) 0.049(4) 0.006(3) 0.006(3) 0.007(3)
C42 0.062(5) 0.076(4) 0.062(5) -0.002(4) 0.020(4) -0.010(4)
C43 0.048(5) 0.125(7) 0.102(7) 0.002(6) 0.012(5) -0.029(4)
C44 0.066(6) 0.109(7) 0.126(9) 0.021(6) 0.046(6) -0.002(5)
C45 0.083(6) 0.128(7) 0.087(6) -0.007(5) 0.049(5) -0.010(5)
C46 0.048(5) 0.095(5) 0.073(5) -0.015(4) 0.028(4) -0.007(4)
C47 0.033(3) 0.042(3) 0.043(4) -0.004(3) 0.011(3) 0.005(3)
C48 0.065(4) 0.050(4) 0.036(4) 0.003(3) 0.011(3) 0.003(3)
C49 0.096(6) 0.067(4) 0.038(4) 0.011(3) 0.015(4) 0.007(4)
C50 0.079(5) 0.090(5) 0.039(4) -0.004(4) 0.012(4) 0.007(4)
C51 0.079(5) 0.067(5) 0.060(5) -0.028(4) 0.024(4) 0.008(4)
C52 0.061(4) 0.044(4) 0.049(4) -0.005(3) 0.006(3) 0.007(3)
C53 0.052(4) 0.031(3) 0.034(3) -0.001(2) 0.003(3) 0.009(3)
C54 0.053(4) 0.043(4) 0.087(5) 0.009(3) 0.023(4) 0.009(3)
C55 0.069(5) 0.043(4) 0.121(7) 0.011(4) 0.035(5) -0.004(4)
C56 0.056(5) 0.069(5) 0.101(6) 0.011(4) 0.029(4) -0.002(4)
C57 0.057(5) 0.050(4) 0.092(6) -0.010(4) 0.032(4) 0.008(3)
C58 0.050(4) 0.040(4) 0.073(5) -0.012(3) 0.017(4) 0.002(3)
C59 0.044(4) 0.040(3) 0.039(4) -0.008(3) 0.009(3) 0.009(3)
C60 0.047(5) 0.109(6) 0.053(5) -0.019(4) 0.003(4) -0.001(4)
C61 0.069(6) 0.144(7) 0.065(6) -0.015(5) 0.029(5) -0.015(5)
C62 0.073(6) 0.116(6) 0.043(5) -0.021(4) 0.009(4) 0.002(5)
C63 0.058(5) 0.092(5) 0.044(5) -0.025(4) 0.000(4) -0.003(4)
C64 0.052(4) 0.059(4) 0.047(4) -0.007(3) 0.007(3) 0.002(3)
C65 0.039(4) 0.042(4) 0.034(3) -0.003(3) 0.007(3) 0.009(3)
C66 0.042(4) 0.043(4) 0.029(3) -0.002(3) 0.003(3) 0.006(3)
C67 0.065(5) 0.070(5) 0.087(6) -0.020(4) 0.013(4) -0.012(4)
C68 0.110(7) 0.109(6) 0.061(5) -0.033(4) -0.019(5) 0.037(5)
N1S 0.127(6) 0.105(5) 0.093(5) -0.025(4) 0.032(5) 0.011(4)
N2S 0.137(8) 0.127(6) 0.133(8) 0.000(5) 0.028(5) -0.037(6)
N3S 0.189(14) 0.120(11) 0.126(11) -0.032(10) 0.009(12) 0.009(10)
C1S 0.166(9) 0.243(11) 0.153(9) -0.112(8) 0.048(7) 0.010(8)
C2S 0.095(6) 0.102(6) 0.097(7) -0.035(5) 0.017(5) 0.010(5)
C3S 0.194(12) 0.293(13) 0.192(12) 0.080(10) 0.088(8) 0.046(10)
C4S 0.120(9) 0.152(8) 0.137(10) 0.034(8) 0.025(6) 0.000(7)
C5S 0.172(15) 0.135(13) 0.155(11) 0.016(12) 0.043(13) 0.022(12)
C6S 0.158(14) 0.126(13) 0.136(11) -0.033(11) 0.046(12) 0.047(11)

_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 O5 1.919(4) . ?
Os1 N2 1.998(4) . ?
Os1 N1 2.000(4) . ?
Os1 O1 2.002(3) . ?
Os1 O2 2.003(3) . ?
Os1 N5 2.045(4) . ?
Os2 O6 1.902(4) . ?
Os2 N3 1.978(5) . ?
Os2 O3 1.999(4) . ?
Os2 N4 2.006(5) . ?
Os2 O4 2.009(4) . ?
Os2 N6 2.058(4) . ?
P1 N5 1.601(4) . ?
P1 C47 1.771(5) . ?
P1 C41 1.773(6) . ?
P1 C65 1.780(6) . ?
P2 N6 1.590(4) . ?
P2 C66 1.766(6) . ?
P2 C53 1.772(6) . ?
P2 C59 1.781(6) . ?
P3 F5 1.467(5) . ?
P3 F3 1.528(5) . ?
P3 F2 1.531(5) . ?
P3 F4 1.536(6) . ?
P3 F6 1.545(5) . ?
P3 F1 1.567(5) . ?
P4 F11 1.507(7) . ?
P4 F12 1.507(7) . ?
P4 F9 1.510(6) . ?
P4 F8 1.557(7) . ?
P4 F7 1.574(7) . ?
P4 F10 1.587(8) . ?
O1 C1 1.326(6) . ?
O2 C20 1.299(6) . ?
O3 C21 1.298(7) . ?
O4 C40 1.319(7) . ?
O5 C67 1.405(6) . ?
O6 C68 1.427(7) . ?
N1 C7 1.297(6) . ?
N1 C8 1.479(6) . ?
N2 C14 1.262(7) . ?
N2 C13 1.472(6) . ?
N3 C27 1.272(7) . ?
N3 C28B 1.431(13) . ?
N3 C28A 1.574(12) . ?
N4 C34 1.269(7) . ?
N4 C33A 1.456(12) . ?
N4 C33B 1.530(14) . ?
N5 H5 0.8600 . ?
N6 H6 0.8600 . ?
C1 C2 1.394(7) . ?
C1 C6 1.427(7) . ?
C2 C3 1.368(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.344(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(7) . ?
C5 H5A 0.9300 . ?
C6 C7 1.415(7) . ?
C7 H7 0.9300 . ?
C8 C13 1.504(8) . ?
C8 C9 1.523(7) . ?
C8 H8 0.9800 . ?
C9 C10 1.516(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.476(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.512(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.496(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13 0.9800 . ?
C14 C15 1.431(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.387(8) . ?
C15 C20 1.427(7) . ?
C16 C17 1.354(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.382(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.358(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.388(8) . ?
C19 H19 0.9300 . ?
C21 C22 1.407(8) . ?
C21 C26 1.427(8) . ?
C22 C23 1.365(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.379(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.366(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.395(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.437(8) . ?
C27 H27 0.9300 . ?
C28A C29A 1.527(13) . ?
C28A C33A 1.545(13) . ?
C28A H28A 0.9800 . ?
C29A C30A 1.490(13) . ?
C29A H29A 0.9700 . ?
C29A H29B 0.9700 . ?
C30A C31A 1.517(14) . ?
C30A H30A 0.9700 . ?
C30A H30B 0.9700 . ?
C31A C32A 1.555(15) . ?
C31A H31A 0.9700 . ?
C31A H31B 0.9700 . ?
C32A C33A 1.572(14) . ?
C32A H32A 0.9700 . ?
C32A H32B 0.9700 . ?
C33A H33A 0.9800 . ?
C28B C33B 1.496(14) . ?
C28B C29B 1.518(14) . ?
C28B H28B 0.9800 . ?
C29B C30B 1.545(14) . ?
C29B H29C 0.9700 . ?
C29B H29D 0.9700 . ?
C30B C31B 1.520(15) . ?
C30B H30C 0.9700 . ?
C30B H30D 0.9700 . ?
C31B C32B 1.536(16) . ?
C31B H31C 0.9700 . ?
C31B H31D 0.9700 . ?
C32B C33B 1.526(15) . ?
C32B H32C 0.9700 . ?
C32B H32D 0.9700 . ?
C33B H33B 0.9800 . ?
C34 C35 1.434(8) . ?
C34 H34 0.9300 . ?
C35 C40 1.398(8) . ?
C35 C36 1.416(9) . ?
C36 C37 1.340(9) . ?
C36 H36 0.9300 . ?
C37 C38 1.391(10) . ?
C37 H37 0.9300 . ?
C38 C39 1.363(9) . ?
C38 H38 0.9300 . ?
C39 C40 1.411(8) . ?
C39 H39 0.9300 . ?
C41 C46 1.373(8) . ?
C41 C42 1.390(8) . ?
C42 C43 1.379(9) . ?
C42 H42 0.9300 . ?
C43 C44 1.334(10) . ?
C43 H43 0.9300 . ?
C44 C45 1.380(10) . ?
C44 H44 0.9300 . ?
C45 C46 1.358(9) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C47 C48 1.382(7) . ?
C47 C52 1.393(7) . ?
C48 C49 1.374(7) . ?
C48 H48 0.9300 . ?
C49 C50 1.372(8) . ?
C49 H49 0.9300 . ?
C50 C51 1.370(8) . ?
C50 H50 0.9300 . ?
C51 C52 1.369(8) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
C53 C58 1.371(7) . ?
C53 C54 1.380(7) . ?
C54 C55 1.371(8) . ?
C54 H54 0.9300 . ?
C55 C56 1.361(8) . ?
C55 H55 0.9300 . ?
C56 C57 1.358(8) . ?
C56 H56 0.9300 . ?
C57 C58 1.369(8) . ?
C57 H57 0.9300 . ?
C58 H58 0.9300 . ?
C59 C60 1.365(8) . ?
C59 C64 1.381(7) . ?
C60 C61 1.388(9) . ?
C60 H60 0.9300 . ?
C61 C62 1.354(9) . ?
C61 H61 0.9300 . ?
C62 C63 1.334(8) . ?
C62 H62 0.9300 . ?
C63 C64 1.371(8) . ?
C63 H63 0.9300 . ?
C64 H64 0.9300 . ?
C65 C66 1.184(6) . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
N1S C2S 1.064(8) . ?
N2S C4S 1.070(12) . ?
N3S C6S 1.11(2) . ?
C1S C2S 1.467(11) . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
C3S C4S 1.444(14) . ?
C3S H3S1 0.9600 . ?
C3S H3S2 0.9600 . ?
C3S H3S3 0.9600 . ?
C5S C6S 1.375(17) . ?
C5S H5S1 0.9600 . ?
C5S H5S2 0.9600 . ?
C5S H5S3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Os1 N2 89.16(17) . . ?
O5 Os1 N1 89.33(16) . . ?
N2 Os1 N1 82.78(17) . . ?
O5 Os1 O1 93.08(15) . . ?
N2 Os1 O1 175.90(16) . . ?
N1 Os1 O1 93.81(15) . . ?
O5 Os1 O2 92.15(15) . . ?
N2 Os1 O2 92.95(16) . . ?
N1 Os1 O2 175.47(16) . . ?
O1 Os1 O2 90.39(13) . . ?
O5 Os1 N5 178.17(17) . . ?
N2 Os1 N5 89.14(17) . . ?
N1 Os1 N5 91.13(17) . . ?
O1 Os1 N5 88.66(15) . . ?
O2 Os1 N5 87.26(15) . . ?
O6 Os2 N3 90.18(18) . . ?
O6 Os2 O3 91.97(17) . . ?
N3 Os2 O3 93.97(19) . . ?
O6 Os2 N4 88.32(19) . . ?
N3 Os2 N4 83.5(2) . . ?
O3 Os2 N4 177.49(19) . . ?
O6 Os2 O4 91.25(16) . . ?
N3 Os2 O4 176.25(19) . . ?
O3 Os2 O4 89.45(16) . . ?
N4 Os2 O4 93.04(19) . . ?
O6 Os2 N6 178.11(16) . . ?
N3 Os2 N6 88.20(17) . . ?
O3 Os2 N6 89.11(16) . . ?
N4 Os2 N6 90.53(17) . . ?
O4 Os2 N6 90.31(15) . . ?
N5 P1 C47 114.9(2) . . ?
N5 P1 C41 107.7(2) . . ?
C47 P1 C41 109.8(3) . . ?
N5 P1 C65 113.5(2) . . ?
C47 P1 C65 104.5(2) . . ?
C41 P1 C65 106.2(3) . . ?
N6 P2 C66 112.6(2) . . ?
N6 P2 C53 115.4(2) . . ?
C66 P2 C53 105.1(2) . . ?
N6 P2 C59 108.1(2) . . ?
C66 P2 C59 106.6(2) . . ?
C53 P2 C59 108.6(3) . . ?
F5 P3 F3 177.8(4) . . ?
F5 P3 F2 91.7(5) . . ?
F3 P3 F2 87.5(4) . . ?
F5 P3 F4 92.4(5) . . ?
F3 P3 F4 88.5(5) . . ?
F2 P3 F4 175.7(5) . . ?
F5 P3 F6 93.2(4) . . ?
F3 P3 F6 88.9(3) . . ?
F2 P3 F6 92.5(3) . . ?
F4 P3 F6 86.1(4) . . ?
F5 P3 F1 91.1(4) . . ?
F3 P3 F1 86.8(3) . . ?
F2 P3 F1 87.8(3) . . ?
F4 P3 F1 93.3(4) . . ?
F6 P3 F1 175.6(4) . . ?
F11 P4 F12 86.8(5) . . ?
F11 P4 F9 171.0(7) . . ?
F12 P4 F9 97.3(6) . . ?
F11 P4 F8 101.7(6) . . ?
F12 P4 F8 92.1(6) . . ?
F9 P4 F8 86.2(4) . . ?
F11 P4 F7 84.2(5) . . ?
F12 P4 F7 170.8(5) . . ?
F9 P4 F7 91.9(5) . . ?
F8 P4 F7 87.7(4) . . ?
F11 P4 F10 87.8(6) . . ?
F12 P4 F10 92.0(5) . . ?
F9 P4 F10 84.1(4) . . ?
F8 P4 F10 169.9(5) . . ?
F7 P4 F10 89.7(5) . . ?
C1 O1 Os1 123.6(3) . . ?
C20 O2 Os1 122.7(3) . . ?
C21 O3 Os2 124.1(4) . . ?
C40 O4 Os2 123.2(4) . . ?
C67 O5 Os1 119.2(3) . . ?
C68 O6 Os2 120.1(4) . . ?
C7 N1 C8 123.2(4) . . ?
C7 N1 Os1 123.9(3) . . ?
C8 N1 Os1 112.8(4) . . ?
C14 N2 C13 124.3(4) . . ?
C14 N2 Os1 124.4(4) . . ?
C13 N2 Os1 111.2(4) . . ?
C27 N3 C28B 115.1(7) . . ?
C27 N3 C28A 127.2(6) . . ?
C28B N3 C28A 27.7(6) . . ?
C27 N3 Os2 125.1(4) . . ?
C28B N3 Os2 117.8(6) . . ?
C28A N3 Os2 106.7(5) . . ?
C34 N4 C33A 119.5(6) . . ?
C34 N4 C33B 125.6(6) . . ?
C33A N4 C33B 27.3(7) . . ?
C34 N4 Os2 125.3(4) . . ?
C33A N4 Os2 114.3(5) . . ?
C33B N4 Os2 106.6(6) . . ?
P1 N5 Os1 129.9(2) . . ?
P1 N5 H5 115.1 . . ?
Os1 N5 H5 115.1 . . ?
P2 N6 Os2 132.0(2) . . ?
P2 N6 H6 114.0 . . ?
Os2 N6 H6 114.0 . . ?
O1 C1 C2 116.5(5) . . ?
O1 C1 C6 125.5(5) . . ?
C2 C1 C6 118.0(5) . . ?
C3 C2 C1 121.8(5) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 120.2(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 119.0(5) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 123.5(5) . . ?
C4 C5 H5A 118.2 . . ?
C6 C5 H5A 118.2 . . ?
C5 C6 C7 117.8(5) . . ?
C5 C6 C1 117.5(5) . . ?
C7 C6 C1 124.6(5) . . ?
N1 C7 C6 127.4(5) . . ?
N1 C7 H7 116.3 . . ?
C6 C7 H7 116.3 . . ?
N1 C8 C13 108.5(5) . . ?
N1 C8 C9 115.6(5) . . ?
C13 C8 C9 112.9(5) . . ?
N1 C8 H8 106.4 . . ?
C13 C8 H8 106.4 . . ?
C9 C8 H8 106.4 . . ?
C10 C9 C8 110.6(5) . . ?
C10 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 C9 114.2(6) . . ?
C11 C10 H10A 108.7 . . ?
C9 C10 H10A 108.7 . . ?
C11 C10 H10B 108.7 . . ?
C9 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C10 C11 C12 114.1(6) . . ?
C10 C11 H11A 108.7 . . ?
C12 C11 H11A 108.7 . . ?
C10 C11 H11B 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C13 C12 C11 110.9(5) . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N2 C13 C12 118.7(5) . . ?
N2 C13 C8 108.0(4) . . ?
C12 C13 C8 113.4(5) . . ?
N2 C13 H13 105.2 . . ?
C12 C13 H13 105.2 . . ?
C8 C13 H13 105.2 . . ?
N2 C14 C15 125.9(5) . . ?
N2 C14 H14 117.0 . . ?
C15 C14 H14 117.0 . . ?
C16 C15 C20 118.4(5) . . ?
C16 C15 C14 117.0(6) . . ?
C20 C15 C14 124.5(5) . . ?
C17 C16 C15 123.1(7) . . ?
C17 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
C16 C17 C18 118.3(8) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
C19 C18 C17 120.8(7) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 122.3(6) . . ?
C18 C19 H19 118.8 . . ?
C20 C19 H19 118.8 . . ?
O2 C20 C19 117.4(5) . . ?
O2 C20 C15 125.5(5) . . ?
C19 C20 C15 117.1(6) . . ?
O3 C21 C22 116.8(6) . . ?
O3 C21 C26 125.4(6) . . ?
C22 C21 C26 117.8(6) . . ?
C23 C22 C21 121.0(7) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 122.3(8) . . ?
C22 C23 H23 118.9 . . ?
C24 C23 H23 118.9 . . ?
C25 C24 C23 117.1(8) . . ?
C25 C24 H24 121.4 . . ?
C23 C24 H24 121.4 . . ?
C24 C25 C26 124.0(7) . . ?
C24 C25 H25 118.0 . . ?
C26 C25 H25 118.0 . . ?
C25 C26 C21 117.7(6) . . ?
C25 C26 C27 117.2(6) . . ?
C21 C26 C27 125.0(6) . . ?
N3 C27 C26 125.9(6) . . ?
N3 C27 H27 117.0 . . ?
C26 C27 H27 117.0 . . ?
C29A C28A C33A 107.6(9) . . ?
C29A C28A N3 112.7(9) . . ?
C33A C28A N3 107.2(8) . . ?
C29A C28A H28A 109.8 . . ?
C33A C28A H28A 109.8 . . ?
N3 C28A H28A 109.8 . . ?
C30A C29A C28A 113.5(11) . . ?
C30A C29A H29A 108.9 . . ?
C28A C29A H29A 108.9 . . ?
C30A C29A H29B 108.9 . . ?
C28A C29A H29B 108.9 . . ?
H29A C29A H29B 107.7 . . ?
C29A C30A C31A 110.6(10) . . ?
C29A C30A H30A 109.5 . . ?
C31A C30A H30A 109.5 . . ?
C29A C30A H30B 109.5 . . ?
C31A C30A H30B 109.5 . . ?
H30A C30A H30B 108.1 . . ?
C30A C31A C32A 109.1(13) . . ?
C30A C31A H31A 109.9 . . ?
C32A C31A H31A 109.9 . . ?
C30A C31A H31B 109.9 . . ?
C32A C31A H31B 109.9 . . ?
H31A C31A H31B 108.3 . . ?
C31A C32A C33A 104.8(12) . . ?
C31A C32A H32A 110.8 . . ?
C33A C32A H32A 110.8 . . ?
C31A C32A H32B 110.8 . . ?
C33A C32A H32B 110.8 . . ?
H32A C32A H32B 108.9 . . ?
N4 C33A C28A 100.6(9) . . ?
N4 C33A C32A 114.4(9) . . ?
C28A C33A C32A 106.5(12) . . ?
N4 C33A H33A 111.6 . . ?
C28A C33A H33A 111.6 . . ?
C32A C33A H33A 111.6 . . ?
N3 C28B C33B 103.7(10) . . ?
N3 C28B C29B 118.8(10) . . ?
C33B C28B C29B 121.9(13) . . ?
N3 C28B H28B 103.3 . . ?
C33B C28B H28B 103.3 . . ?
C29B C28B H28B 103.3 . . ?
C28B C29B C30B 107.9(12) . . ?
C28B C29B H29C 110.1 . . ?
C30B C29B H29C 110.1 . . ?
C28B C29B H29D 110.1 . . ?
C30B C29B H29D 110.1 . . ?
H29C C29B H29D 108.4 . . ?
C31B C30B C29B 117.7(13) . . ?
C31B C30B H30C 107.9 . . ?
C29B C30B H30C 107.9 . . ?
C31B C30B H30D 107.9 . . ?
C29B C30B H30D 107.9 . . ?
H30C C30B H30D 107.2 . . ?
C30B C31B C32B 112.8(13) . . ?
C30B C31B H31C 109.0 . . ?
C32B C31B H31C 109.0 . . ?
C30B C31B H31D 109.0 . . ?
C32B C31B H31D 109.0 . . ?
H31C C31B H31D 107.8 . . ?
C33B C32B C31B 112.9(15) . . ?
C33B C32B H32C 109.0 . . ?
C31B C32B H32C 109.0 . . ?
C33B C32B H32D 109.0 . . ?
C31B C32B H32D 109.0 . . ?
H32C C32B H32D 107.8 . . ?
C28B C33B C32B 110.0(12) . . ?
C28B C33B N4 114.6(10) . . ?
C32B C33B N4 115.6(12) . . ?
C28B C33B H33B 105.2 . . ?
C32B C33B H33B 105.2 . . ?
N4 C33B H33B 105.2 . . ?
N4 C34 C35 125.8(6) . . ?
N4 C34 H34 117.1 . . ?
C35 C34 H34 117.1 . . ?
C40 C35 C36 118.5(6) . . ?
C40 C35 C34 125.4(6) . . ?
C36 C35 C34 116.1(6) . . ?
C37 C36 C35 123.3(7) . . ?
C37 C36 H36 118.4 . . ?
C35 C36 H36 118.4 . . ?
C36 C37 C38 117.6(8) . . ?
C36 C37 H37 121.2 . . ?
C38 C37 H37 121.2 . . ?
C39 C38 C37 122.0(7) . . ?
C39 C38 H38 119.0 . . ?
C37 C38 H38 119.0 . . ?
C38 C39 C40 120.6(7) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 H39 119.7 . . ?
O4 C40 C35 126.2(6) . . ?
O4 C40 C39 115.8(6) . . ?
C35 C40 C39 118.0(6) . . ?
C46 C41 C42 118.1(6) . . ?
C46 C41 P1 120.0(5) . . ?
C42 C41 P1 121.4(5) . . ?
C43 C42 C41 120.4(7) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C44 C43 C42 120.2(8) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 120.3(8) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C46 C45 C44 120.0(8) . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C45 C46 C41 120.9(7) . . ?
C45 C46 H46 119.6 . . ?
C41 C46 H46 119.6 . . ?
C48 C47 C52 118.1(5) . . ?
C48 C47 P1 122.6(4) . . ?
C52 C47 P1 119.2(4) . . ?
C49 C48 C47 120.8(5) . . ?
C49 C48 H48 119.6 . . ?
C47 C48 H48 119.6 . . ?
C50 C49 C48 120.2(6) . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
C51 C50 C49 119.9(6) . . ?
C51 C50 H50 120.1 . . ?
C49 C50 H50 120.1 . . ?
C50 C51 C52 120.1(6) . . ?
C50 C51 H51 119.9 . . ?
C52 C51 H51 119.9 . . ?
C51 C52 C47 120.9(5) . . ?
C51 C52 H52 119.6 . . ?
C47 C52 H52 119.6 . . ?
C58 C53 C54 118.5(5) . . ?
C58 C53 P2 123.3(4) . . ?
C54 C53 P2 118.1(4) . . ?
C55 C54 C53 120.7(5) . . ?
C55 C54 H54 119.7 . . ?
C53 C54 H54 119.7 . . ?
C56 C55 C54 120.1(6) . . ?
C56 C55 H55 120.0 . . ?
C54 C55 H55 120.0 . . ?
C57 C56 C55 119.5(6) . . ?
C57 C56 H56 120.2 . . ?
C55 C56 H56 120.2 . . ?
C56 C57 C58 121.0(6) . . ?
C56 C57 H57 119.5 . . ?
C58 C57 H57 119.5 . . ?
C57 C58 C53 120.2(5) . . ?
C57 C58 H58 119.9 . . ?
C53 C58 H58 119.9 . . ?
C60 C59 C64 118.9(6) . . ?
C60 C59 P2 118.8(5) . . ?
C64 C59 P2 122.1(5) . . ?
C59 C60 C61 119.7(6) . . ?
C59 C60 H60 120.1 . . ?
C61 C60 H60 120.1 . . ?
C62 C61 C60 120.2(7) . . ?
C62 C61 H61 119.9 . . ?
C60 C61 H61 119.9 . . ?
C63 C62 C61 120.2(7) . . ?
C63 C62 H62 119.9 . . ?
C61 C62 H62 119.9 . . ?
C62 C63 C64 121.0(6) . . ?
C62 C63 H63 119.5 . . ?
C64 C63 H63 119.5 . . ?
C63 C64 C59 119.9(6) . . ?
C63 C64 H64 120.1 . . ?
C59 C64 H64 120.1 . . ?
C66 C65 P1 173.9(5) . . ?
C65 C66 P2 174.1(5) . . ?
O5 C67 H67A 109.5 . . ?
O5 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
O5 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
O6 C68 H68A 109.5 . . ?
O6 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
O6 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
N1S C2S C1S 179.1(12) . . ?
C4S C3S H3S1 109.5 . . ?
C4S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
C4S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
N2S C4S C3S 178.4(16) . . ?
C6S C5S H5S1 109.5 . . ?
C6S C5S H5S2 109.5 . . ?
H5S1 C5S H5S2 109.5 . . ?
C6S C5S H5S3 109.5 . . ?
H5S1 C5S H5S3 109.5 . . ?
H5S2 C5S H5S3 109.5 . . ?
N3S C6S C5S 162(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.085

data_7
_database_code_depnum_ccdc_archive 'CCDC 793802'
#TrackingRef '- Os(salen)binuclear.Dalton(CIF).cif'

# wt0744w-TCLau292-TCL-CY1_12-4-2001

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H56 Cl2 Fe N6 O4 Os2 P2'
_chemical_formula_sum            'C74 H56 Cl2 Fe N6 O4 Os2 P2'
_chemical_formula_weight         1662.34

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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   11.698(4)
_cell_length_b                   12.230(4)
_cell_length_c                   13.216(4)
_cell_angle_alpha                85.212(6)
_cell_angle_beta                 69.354(5)
_cell_angle_gamma                64.352(5)
_cell_volume                     1589.7(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9882
_cell_measurement_theta_min      1.65
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    4.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6201
_exptl_absorpt_correction_T_max  0.8435
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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 1000 CCD Detector'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9882
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         27.53
_reflns_number_total             6872
_reflns_number_gt                5546
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'SMART (Bruker AXS Inc., 1998)'
_computing_cell_refinement       'SAINT (Bruker AXS Inc.,1999)'
_computing_data_reduction        
'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976) & Mercury'
_computing_publication_material  SHELXL-97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0431P)^2^] where P=(Fo^2^+2Fc^2^)/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         6872
_refine_ls_number_parameters     413
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0836
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_restrained_S_all      0.968
_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
Os1 Os 0.613266(19) 0.204648(17) 0.800952(17) 0.02922(7) Uani 1 1 d . . .
Fe1 Fe 0.5000 0.5000 0.5000 0.0287(2) Uani 1 2 d S . .
Cl1 Cl 0.77775(15) 0.04952(13) 0.86721(13) 0.0505(4) Uani 1 1 d . . .
P1 P 0.34790(13) 0.40273(12) 0.73066(11) 0.0300(3) Uani 1 1 d . . .
O1 O 0.5452(3) 0.3119(3) 0.9372(3) 0.0344(8) Uani 1 1 d . . .
O2 O 0.7531(3) 0.2712(3) 0.7320(3) 0.0372(8) Uani 1 1 d . . .
N1 N 0.4912(4) 0.1222(4) 0.8652(3) 0.0308(9) Uani 1 1 d . . .
N2 N 0.6780(4) 0.0904(4) 0.6725(4) 0.0335(10) Uani 1 1 d . . .
N3 N 0.4822(4) 0.3276(4) 0.7532(3) 0.0337(10) Uani 1 1 d . . .
C1 C 0.4339(5) 0.3254(5) 1.0197(4) 0.0334(11) Uani 1 1 d . . .
C2 C 0.3818(6) 0.4206(5) 1.0989(5) 0.0439(14) Uani 1 1 d . . .
H2 H 0.4247 0.4712 1.0902 0.053 Uiso 1 1 calc R . .
C3 C 0.2686(6) 0.4408(6) 1.1893(5) 0.0574(17) Uani 1 1 d . . .
H3 H 0.2365 0.5046 1.2406 0.069 Uiso 1 1 calc R . .
C4 C 0.2010(7) 0.3673(7) 1.2051(6) 0.069(2) Uani 1 1 d . . .
H4 H 0.1249 0.3812 1.2667 0.083 Uiso 1 1 calc R . .
C5 C 0.2482(6) 0.2750(6) 1.1293(5) 0.0587(18) Uani 1 1 d . . .
H5 H 0.2035 0.2256 1.1403 0.070 Uiso 1 1 calc R . .
C6 C 0.3635(5) 0.2511(5) 1.0336(4) 0.0400(13) Uani 1 1 d . . .
C7 C 0.3971(5) 0.1539(5) 0.9604(4) 0.0396(13) Uani 1 1 d . . .
H7 H 0.3469 0.1089 0.9829 0.048 Uiso 1 1 calc R . .
C8 C 0.5143(5) 0.0278(5) 0.7929(5) 0.0367(12) Uani 1 1 d . . .
C9 C 0.4482(6) -0.0474(5) 0.8195(5) 0.0509(15) Uani 1 1 d . . .
H9 H 0.3861 -0.0399 0.8889 0.061 Uiso 1 1 calc R . .
C10 C 0.4750(7) -0.1325(7) 0.7427(6) 0.070(2) Uani 1 1 d . . .
H10 H 0.4311 -0.1829 0.7605 0.084 Uiso 1 1 calc R . .
C11 C 0.5664(7) -0.1440(6) 0.6396(6) 0.070(2) Uani 1 1 d . . .
H11 H 0.5830 -0.2018 0.5884 0.084 Uiso 1 1 calc R . .
C12 C 0.6336(6) -0.0714(6) 0.6113(5) 0.0556(17) Uani 1 1 d . . .
H12 H 0.6943 -0.0790 0.5412 0.067 Uiso 1 1 calc R . .
C13 C 0.6098(5) 0.0137(5) 0.6888(4) 0.0370(12) Uani 1 1 d . . .
C14 C 0.7700(5) 0.0879(5) 0.5785(4) 0.0357(12) Uani 1 1 d . . .
H14 H 0.7880 0.0352 0.5222 0.043 Uiso 1 1 calc R . .
C15 C 0.8443(5) 0.1594(5) 0.5558(4) 0.0352(12) Uani 1 1 d . . .
C16 C 0.9370(5) 0.1416(5) 0.4472(5) 0.0426(13) Uani 1 1 d . . .
H16 H 0.9397 0.0903 0.3974 0.051 Uiso 1 1 calc R . .
C17 C 1.0211(6) 0.1968(5) 0.4137(5) 0.0468(15) Uani 1 1 d . . .
H17 H 1.0788 0.1851 0.3419 0.056 Uiso 1 1 calc R . .
C18 C 1.0194(6) 0.2713(5) 0.4891(5) 0.0502(16) Uani 1 1 d . . .
H18 H 1.0783 0.3080 0.4674 0.060 Uiso 1 1 calc R . .
C19 C 0.9321(5) 0.2914(5) 0.5949(5) 0.0449(14) Uani 1 1 d . . .
H19 H 0.9351 0.3396 0.6439 0.054 Uiso 1 1 calc R . .
C20 C 0.8381(5) 0.2408(4) 0.6311(4) 0.0346(12) Uani 1 1 d . . .
C21 C 0.3871(5) 0.4145(4) 0.5874(4) 0.0310(11) Uani 1 1 d . . .
C22 C 0.5123(5) 0.3290(4) 0.5105(4) 0.0356(12) Uani 1 1 d . . .
H22 H 0.5783 0.2613 0.5271 0.043 Uiso 1 1 calc R . .
C23 C 0.5174(6) 0.3657(5) 0.4061(4) 0.0398(13) Uani 1 1 d . . .
H23 H 0.5883 0.3269 0.3418 0.048 Uiso 1 1 calc R . .
C24 C 0.3973(6) 0.4710(5) 0.4149(4) 0.0417(13) Uani 1 1 d . . .
H24 H 0.3751 0.5127 0.3574 0.050 Uiso 1 1 calc R . .
C25 C 0.3167(6) 0.5023(5) 0.5258(5) 0.0384(12) Uani 1 1 d . . .
H25 H 0.2325 0.5684 0.5541 0.046 Uiso 1 1 calc R . .
C26 C 0.2628(5) 0.5548(4) 0.7975(4) 0.0317(11) Uani 1 1 d . . .
C27 C 0.1464(5) 0.6457(5) 0.7817(5) 0.0425(13) Uani 1 1 d . . .
H27 H 0.1043 0.6273 0.7421 0.051 Uiso 1 1 calc R . .
C28 C 0.0961(6) 0.7628(5) 0.8263(5) 0.0512(16) Uani 1 1 d . . .
H28 H 0.0217 0.8243 0.8137 0.061 Uiso 1 1 calc R . .
C29 C 0.1538(6) 0.7900(5) 0.8886(5) 0.0526(16) Uani 1 1 d . . .
H29 H 0.1179 0.8694 0.9180 0.063 Uiso 1 1 calc R . .
C30 C 0.2645(6) 0.7007(5) 0.9082(5) 0.0462(14) Uani 1 1 d . . .
H30 H 0.3022 0.7190 0.9520 0.055 Uiso 1 1 calc R . .
C31 C 0.3192(5) 0.5832(5) 0.8618(4) 0.0372(12) Uani 1 1 d . . .
H31 H 0.3945 0.5228 0.8739 0.045 Uiso 1 1 calc R . .
C32 C 0.2274(5) 0.3376(5) 0.7713(4) 0.0353(12) Uani 1 1 d . . .
C33 C 0.1142(7) 0.3813(7) 0.8647(6) 0.070(2) Uani 1 1 d . . .
H33 H 0.0984 0.4457 0.9085 0.084 Uiso 1 1 calc R . .
C34 C 0.0245(8) 0.3295(8) 0.8930(7) 0.091(3) Uani 1 1 d . . .
H34 H -0.0540 0.3619 0.9539 0.109 Uiso 1 1 calc R . .
C35 C 0.0500(8) 0.2304(8) 0.8321(7) 0.080(2) Uani 1 1 d . . .
H35 H -0.0101 0.1950 0.8524 0.096 Uiso 1 1 calc R . .
C36 C 0.1625(8) 0.1849(7) 0.7429(6) 0.072(2) Uani 1 1 d . . .
H36 H 0.1810 0.1170 0.7020 0.086 Uiso 1 1 calc R . .
C37 C 0.2508(6) 0.2392(6) 0.7118(5) 0.0561(17) Uani 1 1 d . . .
H37 H 0.3273 0.2080 0.6492 0.067 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os1 0.02859(11) 0.02529(10) 0.03116(12) 0.00546(7) -0.01002(8) -0.01030(8)
Fe1 0.0360(5) 0.0258(5) 0.0274(5) 0.0065(4) -0.0126(4) -0.0156(4)
Cl1 0.0444(8) 0.0391(8) 0.0630(10) 0.0131(7) -0.0284(7) -0.0078(6)
P1 0.0296(7) 0.0298(7) 0.0289(7) 0.0071(5) -0.0092(5) -0.0130(5)
O1 0.0341(19) 0.0342(19) 0.036(2) 0.0022(16) -0.0097(16) -0.0170(16)
O2 0.0314(19) 0.036(2) 0.043(2) 0.0020(17) -0.0101(17) -0.0158(16)
N1 0.035(2) 0.030(2) 0.029(2) 0.0077(18) -0.0131(19) -0.0157(18)
N2 0.035(2) 0.024(2) 0.041(3) 0.0025(18) -0.014(2) -0.0122(18)
N3 0.031(2) 0.033(2) 0.032(2) -0.0005(18) -0.0099(19) -0.0108(19)
C1 0.034(3) 0.034(3) 0.029(3) 0.005(2) -0.013(2) -0.011(2)
C2 0.051(3) 0.043(3) 0.041(3) -0.002(3) -0.013(3) -0.025(3)
C3 0.058(4) 0.063(4) 0.042(4) -0.015(3) -0.003(3) -0.026(3)
C4 0.064(5) 0.084(5) 0.044(4) -0.014(4) 0.012(3) -0.040(4)
C5 0.059(4) 0.068(4) 0.046(4) -0.001(3) 0.001(3) -0.039(4)
C6 0.042(3) 0.041(3) 0.036(3) 0.006(2) -0.009(2) -0.021(3)
C7 0.044(3) 0.040(3) 0.040(3) 0.006(3) -0.011(3) -0.026(3)
C8 0.039(3) 0.030(3) 0.046(3) 0.006(2) -0.018(3) -0.016(2)
C9 0.060(4) 0.049(4) 0.051(4) 0.009(3) -0.012(3) -0.036(3)
C10 0.081(5) 0.071(5) 0.073(5) -0.004(4) -0.010(4) -0.058(4)
C11 0.088(5) 0.065(5) 0.064(5) -0.012(4) -0.011(4) -0.048(4)
C12 0.061(4) 0.055(4) 0.053(4) -0.013(3) -0.005(3) -0.035(3)
C13 0.037(3) 0.032(3) 0.039(3) 0.001(2) -0.012(2) -0.014(2)
C14 0.037(3) 0.030(3) 0.034(3) -0.001(2) -0.011(2) -0.009(2)
C15 0.029(3) 0.032(3) 0.038(3) 0.007(2) -0.011(2) -0.008(2)
C16 0.042(3) 0.034(3) 0.040(3) 0.006(2) -0.012(3) -0.009(2)
C17 0.039(3) 0.048(3) 0.038(3) 0.011(3) -0.003(3) -0.015(3)
C18 0.034(3) 0.043(3) 0.061(4) 0.010(3) -0.007(3) -0.015(3)
C19 0.033(3) 0.039(3) 0.058(4) 0.000(3) -0.009(3) -0.015(2)
C20 0.024(2) 0.031(3) 0.041(3) 0.005(2) -0.009(2) -0.007(2)
C21 0.036(3) 0.030(3) 0.031(3) 0.007(2) -0.012(2) -0.019(2)
C22 0.044(3) 0.026(3) 0.033(3) 0.000(2) -0.010(2) -0.015(2)
C23 0.057(4) 0.039(3) 0.031(3) 0.003(2) -0.011(3) -0.030(3)
C24 0.060(4) 0.050(3) 0.033(3) 0.014(3) -0.025(3) -0.034(3)
C25 0.040(3) 0.039(3) 0.045(3) 0.013(3) -0.023(3) -0.020(2)
C26 0.029(3) 0.031(3) 0.030(3) 0.008(2) -0.007(2) -0.012(2)
C27 0.035(3) 0.042(3) 0.045(3) 0.003(3) -0.016(3) -0.010(2)
C28 0.047(4) 0.033(3) 0.057(4) 0.006(3) -0.017(3) -0.004(3)
C29 0.058(4) 0.034(3) 0.047(4) -0.003(3) -0.003(3) -0.014(3)
C30 0.047(3) 0.044(3) 0.048(4) 0.000(3) -0.013(3) -0.023(3)
C31 0.036(3) 0.036(3) 0.039(3) 0.006(2) -0.011(2) -0.016(2)
C32 0.036(3) 0.045(3) 0.032(3) 0.010(2) -0.013(2) -0.023(2)
C33 0.078(5) 0.069(5) 0.060(5) -0.008(4) 0.007(4) -0.053(4)
C34 0.083(6) 0.104(7) 0.079(6) -0.005(5) 0.016(5) -0.066(5)
C35 0.080(5) 0.095(6) 0.086(6) 0.029(5) -0.021(5) -0.067(5)
C36 0.088(6) 0.082(5) 0.072(5) 0.012(4) -0.026(5) -0.064(5)
C37 0.055(4) 0.063(4) 0.053(4) 0.000(3) -0.005(3) -0.038(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 N3 1.881(4) . ?
Os1 N2 1.996(4) . ?
Os1 N1 2.007(4) . ?
Os1 O1 2.019(3) . ?
Os1 O2 2.036(3) . ?
Os1 Cl1 2.4123(14) . ?
Fe1 C21 2.022(5) 2_666 ?
Fe1 C21 2.022(5) . ?
Fe1 C22 2.030(5) 2_666 ?
Fe1 C22 2.030(5) . ?
Fe1 C25 2.037(5) 2_666 ?
Fe1 C25 2.037(5) . ?
Fe1 C23 2.038(5) 2_666 ?
Fe1 C23 2.038(5) . ?
Fe1 C24 2.055(5) . ?
Fe1 C24 2.055(5) 2_666 ?
P1 N3 1.561(4) . ?
P1 C21 1.793(5) . ?
P1 C32 1.811(5) . ?
P1 C26 1.812(5) . ?
O1 C1 1.325(6) . ?
O2 C20 1.317(6) . ?
N1 C7 1.296(6) . ?
N1 C8 1.432(6) . ?
N2 C14 1.318(6) . ?
N2 C13 1.433(6) . ?
C1 C2 1.400(7) . ?
C1 C6 1.432(7) . ?
C2 C3 1.376(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.395(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.357(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.422(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.423(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.392(7) . ?
C8 C13 1.401(7) . ?
C9 C10 1.371(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.376(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.374(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.391(7) . ?
C12 H12 0.9300 . ?
C14 C15 1.429(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.426(7) . ?
C15 C20 1.427(7) . ?
C16 C17 1.355(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.395(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.376(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.411(7) . ?
C19 H19 0.9300 . ?
C21 C25 1.433(7) . ?
C21 C22 1.440(7) . ?
C22 C23 1.404(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.411(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.411(8) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C31 1.385(7) . ?
C26 C27 1.409(7) . ?
C27 C28 1.383(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.371(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.379(8) . ?
C29 H29 0.9300 . ?
C30 C31 1.387(7) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 C37 1.365(8) . ?
C32 C33 1.381(8) . ?
C33 C34 1.379(9) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(11) . ?
C34 H34 0.9300 . ?
C35 C36 1.347(11) . ?
C35 H35 0.9300 . ?
C36 C37 1.388(8) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?

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 Os1 N2 92.45(17) . . ?
N3 Os1 N1 91.59(17) . . ?
N2 Os1 N1 82.17(17) . . ?
N3 Os1 O1 89.55(16) . . ?
N2 Os1 O1 176.24(15) . . ?
N1 Os1 O1 94.59(15) . . ?
N3 Os1 O2 93.19(16) . . ?
N2 Os1 O2 94.33(16) . . ?
N1 Os1 O2 174.20(14) . . ?
O1 Os1 O2 88.74(14) . . ?
N3 Os1 Cl1 178.42(13) . . ?
N2 Os1 Cl1 89.00(13) . . ?
N1 Os1 Cl1 88.01(12) . . ?
O1 Os1 Cl1 88.96(11) . . ?
O2 Os1 Cl1 87.31(11) . . ?
C21 Fe1 C21 180.0 2_666 . ?
C21 Fe1 C22 41.65(19) 2_666 2_666 ?
C21 Fe1 C22 138.35(19) . 2_666 ?
C21 Fe1 C22 138.35(19) 2_666 . ?
C21 Fe1 C22 41.65(19) . . ?
C22 Fe1 C22 180.000(1) 2_666 . ?
C21 Fe1 C25 41.4(2) 2_666 2_666 ?
C21 Fe1 C25 138.6(2) . 2_666 ?
C22 Fe1 C25 69.1(2) 2_666 2_666 ?
C22 Fe1 C25 110.9(2) . 2_666 ?
C21 Fe1 C25 138.6(2) 2_666 . ?
C21 Fe1 C25 41.4(2) . . ?
C22 Fe1 C25 110.9(2) 2_666 . ?
C22 Fe1 C25 69.1(2) . . ?
C25 Fe1 C25 180.0(5) 2_666 . ?
C21 Fe1 C23 69.1(2) 2_666 2_666 ?
C21 Fe1 C23 110.9(2) . 2_666 ?
C22 Fe1 C23 40.4(2) 2_666 2_666 ?
C22 Fe1 C23 139.6(2) . 2_666 ?
C25 Fe1 C23 68.3(2) 2_666 2_666 ?
C25 Fe1 C23 111.7(2) . 2_666 ?
C21 Fe1 C23 110.9(2) 2_666 . ?
C21 Fe1 C23 69.1(2) . . ?
C22 Fe1 C23 139.6(2) 2_666 . ?
C22 Fe1 C23 40.4(2) . . ?
C25 Fe1 C23 111.7(2) 2_666 . ?
C25 Fe1 C23 68.3(2) . . ?
C23 Fe1 C23 180.0(2) 2_666 . ?
C21 Fe1 C24 111.2(2) 2_666 . ?
C21 Fe1 C24 68.8(2) . . ?
C22 Fe1 C24 111.9(2) 2_666 . ?
C22 Fe1 C24 68.1(2) . . ?
C25 Fe1 C24 139.6(2) 2_666 . ?
C25 Fe1 C24 40.4(2) . . ?
C23 Fe1 C24 139.7(2) 2_666 . ?
C23 Fe1 C24 40.3(2) . . ?
C21 Fe1 C24 68.8(2) 2_666 2_666 ?
C21 Fe1 C24 111.2(2) . 2_666 ?
C22 Fe1 C24 68.1(2) 2_666 2_666 ?
C22 Fe1 C24 111.9(2) . 2_666 ?
C25 Fe1 C24 40.4(2) 2_666 2_666 ?
C25 Fe1 C24 139.6(2) . 2_666 ?
C23 Fe1 C24 40.3(2) 2_666 2_666 ?
C23 Fe1 C24 139.7(2) . 2_666 ?
C24 Fe1 C24 180.000(1) . 2_666 ?
N3 P1 C21 109.0(2) . . ?
N3 P1 C32 115.5(2) . . ?
C21 P1 C32 105.5(2) . . ?
N3 P1 C26 110.4(2) . . ?
C21 P1 C26 108.5(2) . . ?
C32 P1 C26 107.7(2) . . ?
C1 O1 Os1 122.4(3) . . ?
C20 O2 Os1 123.4(3) . . ?
C7 N1 C8 123.1(4) . . ?
C7 N1 Os1 123.9(3) . . ?
C8 N1 Os1 113.0(3) . . ?
C14 N2 C13 121.8(4) . . ?
C14 N2 Os1 124.2(4) . . ?
C13 N2 Os1 113.9(3) . . ?
P1 N3 Os1 160.7(3) . . ?
O1 C1 C2 116.7(5) . . ?
O1 C1 C6 125.2(5) . . ?
C2 C1 C6 118.1(5) . . ?
C3 C2 C1 121.4(5) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 121.1(6) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 118.9(6) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 122.4(6) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C7 115.5(5) . . ?
C5 C6 C1 118.1(5) . . ?
C7 C6 C1 126.5(5) . . ?
N1 C7 C6 126.0(5) . . ?
N1 C7 H7 117.0 . . ?
C6 C7 H7 117.0 . . ?
C9 C8 C13 119.6(5) . . ?
C9 C8 N1 124.5(5) . . ?
C13 C8 N1 115.9(4) . . ?
C10 C9 C8 119.7(6) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 120.6(6) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C12 C11 C10 120.9(6) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 119.3(6) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C8 119.8(5) . . ?
C12 C13 N2 125.3(5) . . ?
C8 C13 N2 114.9(5) . . ?
N2 C14 C15 125.5(5) . . ?
N2 C14 H14 117.2 . . ?
C15 C14 H14 117.2 . . ?
C16 C15 C20 118.5(5) . . ?
C16 C15 C14 114.8(5) . . ?
C20 C15 C14 126.6(5) . . ?
C17 C16 C15 122.5(6) . . ?
C17 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
C16 C17 C18 118.8(5) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
C19 C18 C17 121.1(5) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 121.6(6) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
O2 C20 C19 117.2(5) . . ?
O2 C20 C15 125.4(5) . . ?
C19 C20 C15 117.3(5) . . ?
C25 C21 C22 106.7(5) . . ?
C25 C21 P1 132.0(4) . . ?
C22 C21 P1 121.2(4) . . ?
C25 C21 Fe1 69.9(3) . . ?
C22 C21 Fe1 69.5(3) . . ?
P1 C21 Fe1 123.2(3) . . ?
C23 C22 C21 108.0(5) . . ?
C23 C22 Fe1 70.1(3) . . ?
C21 C22 Fe1 68.9(3) . . ?
C23 C22 H22 126.0 . . ?
C21 C22 H22 126.0 . . ?
Fe1 C22 H22 126.6 . . ?
C22 C23 C24 108.8(5) . . ?
C22 C23 Fe1 69.5(3) . . ?
C24 C23 Fe1 70.5(3) . . ?
C22 C23 H23 125.6 . . ?
C24 C23 H23 125.6 . . ?
Fe1 C23 H23 126.0 . . ?
C23 C24 C25 108.3(5) . . ?
C23 C24 Fe1 69.2(3) . . ?
C25 C24 Fe1 69.1(3) . . ?
C23 C24 H24 125.9 . . ?
C25 C24 H24 125.9 . . ?
Fe1 C24 H24 127.4 . . ?
C24 C25 C21 108.2(5) . . ?
C24 C25 Fe1 70.5(3) . . ?
C21 C25 Fe1 68.8(3) . . ?
C24 C25 H25 125.9 . . ?
C21 C25 H25 125.9 . . ?
Fe1 C25 H25 126.4 . . ?
C31 C26 C27 119.5(5) . . ?
C31 C26 P1 118.2(4) . . ?
C27 C26 P1 122.2(4) . . ?
C28 C27 C26 118.6(6) . . ?
C28 C27 H27 120.7 . . ?
C26 C27 H27 120.7 . . ?
C29 C28 C27 121.2(6) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C28 C29 C30 120.6(5) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C29 C30 C31 119.2(6) . . ?
C29 C30 H30 120.4 . . ?
C31 C30 H30 120.4 . . ?
C26 C31 C30 120.8(5) . . ?
C26 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
C37 C32 C33 118.4(5) . . ?
C37 C32 P1 119.9(4) . . ?
C33 C32 P1 121.6(4) . . ?
C34 C33 C32 120.0(7) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C35 C34 C33 120.6(7) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C36 C35 C34 119.6(7) . . ?
C36 C35 H35 120.2 . . ?
C34 C35 H35 120.2 . . ?
C35 C36 C37 120.1(7) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C32 C37 C36 121.1(6) . . ?
C32 C37 H37 119.4 . . ?
C36 C37 H37 119.4 . . ?

_diffrn_measured_fraction_theta_max 0.937
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.937
_refine_diff_density_max         2.824
_refine_diff_density_min         -1.867
_refine_diff_density_rms         0.140

# start Validation Reply Form
_vrf_PLAT029_WT0744W-shelxl      
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.94
RESPONSE: A standard data collection routine was used which supposedly
should have cover the hemisphere data. May be due to the orientation
of the crystal, some of the reflections were not covered for triclinic
primitive space group, thus the fraction of measured data is less than
95%.
;
# end Validation Reply Form