# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cmpnd_1
_database_code_depnum_ccdc_archive 'CCDC 1983330'
loop_
_audit_author_name
_audit_author_address
'Pilar Garcia-Orduna'
;Instituto de Sintesis Quimica y Catalisis Homogenea (ISQCH, CSIC Univ Zaragoza)
Spain
;
_audit_update_record             
;
2020-07-31 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H36 Cl N4 Os, F6 Sb, 1.5(C H4 O)'
_chemical_formula_sum            'C32.50 H42 Cl F6 N4 O1.50 Os Sb'
_chemical_formula_weight         974.10

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8413(6)
_cell_length_b                   11.1473(6)
_cell_length_c                   15.2059(6)
_cell_angle_alpha                92.1850(10)
_cell_angle_beta                 93.7980(10)
_cell_angle_gamma                110.5430(10)
_cell_volume                     1713.31(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7899
_cell_measurement_theta_min      2.250
_cell_measurement_theta_max      28.160

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_F_000             950
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.638
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5093
_exptl_absorpt_correction_T_max  0.6974
_exptl_absorpt_process_details   
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.
;
_exptl_absorpt_special_details   ?



_diffrn_ambient_temperature      100(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 APEX CCD system'
_diffrn_measurement_method       'narrow ω frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21006
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.255
_diffrn_reflns_theta_max         28.621
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7990
_reflns_number_gt                7033
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_cell_refinement       'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'

_refine_special_details          
;Two carbon atoms of methyl groups of p-cymene have been found to be disordered.
They have been included in the model in two sets of positions whit
complementary occupancy factors (0.686/0.314(9)) and isotropically refined.

Although hydrogen atoms have been observed in Fourier difference maps, most
of them have been included in the model in observed positions and refined
with a riding model. Those of N-H fragments have been included in observed
positions and refined with a geometrical restrain in N-H bond lengths.

When convergence is achieved, four residual density peaks bigger than 1 e/A^3 
are found in the intermolecular region. Several test were made to interpret
them as carbon and oxygen atoms of methanol solvent. However, it leads to
unrealistic geometry.

 Therefore, SQUEEZE corrections  have been applied. The total potential solvent 
 accesible void volume (147 A3) and the electron count (49 e in the unit cell) 
 may agree with the presence of three methanol molecules (C H3 O H).They have 
 been included in the chemical formula, F00 and density. Results of the SQUEEZE
 calculations are included below.,SQUEEZE
;

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 147 49 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?



_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0276P)²+1.3390P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Direct method'
_atom_sites_solution_secondary   'Fourier difference synthesis'
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7990
_refine_ls_number_parameters     410
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0633
_refine_ls_wR_factor_gt          0.0599
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.76052(2) 0.67957(2) 0.63443(2) 0.01991(5) Uani 1 1 d . . . . .
Cl Cl 0.70236(8) 0.76469(9) 0.50004(6) 0.02569(19) Uani 1 1 d . . . . .
N1 N 0.6732(3) 0.7973(3) 0.6955(2) 0.0244(7) Uani 1 1 d . . . . .
N2 N 0.9173(3) 0.8569(3) 0.65798(19) 0.0209(6) Uani 1 1 d . . . . .
N3 N 1.0196(3) 0.8449(3) 0.5318(2) 0.0219(6) Uani 1 1 d D . . . .
N4 N 1.1226(3) 1.0143(3) 0.6376(2) 0.0217(6) Uani 1 1 d D . . . .
C1 C 0.7786(4) 0.5129(4) 0.5599(3) 0.0288(9) Uani 1 1 d . . . . .
C2 C 0.8820(4) 0.5597(4) 0.6260(3) 0.0336(10) Uani 1 1 d . . . . .
H2 H 0.970434 0.579740 0.611029 0.040 Uiso 1 1 calc R U . . .
C3 C 0.8581(4) 0.5779(4) 0.7150(3) 0.0347(10) Uani 1 1 d . . . . .
H3 H 0.930856 0.612708 0.758338 0.042 Uiso 1 1 calc R U . . .
C4 C 0.7285(5) 0.5454(4) 0.7406(3) 0.0364(10) Uani 1 1 d . . . . .
C5 C 0.6221(4) 0.4975(4) 0.6735(3) 0.0314(9) Uani 1 1 d . . . . .
H5 H 0.533736 0.476319 0.688700 0.038 Uiso 1 1 calc R U . . .
C6 C 0.6461(4) 0.4813(4) 0.5855(3) 0.0268(8) Uani 1 1 d . . . . .
H6 H 0.573680 0.448859 0.541838 0.032 Uiso 1 1 calc R U . . .
C7 C 0.8036(6) 0.4995(4) 0.4649(3) 0.0477(13) Uani 1 1 d . . . . .
H7A H 0.893840 0.555422 0.455933 0.072 Uiso 1 1 calc R U . . .
H7B H 0.740450 0.524271 0.427487 0.072 Uiso 1 1 calc R U . . .
H7C H 0.792748 0.410141 0.449058 0.072 Uiso 1 1 calc R U . . .
C8A C 0.6814(8) 0.5593(7) 0.8336(5) 0.0387(17) Uiso 0.678(9) 1 d . . P A 1
H8A H 0.592382 0.567721 0.827865 0.046 Uiso 0.678(9) 1 calc R U P A 1
C9A C 0.6728(11) 0.4348(9) 0.8770(6) 0.068(3) Uiso 0.678(9) 1 d . . P A 1
H9A1 H 0.761692 0.431434 0.887213 0.102 Uiso 0.678(9) 1 calc R U P A 1
H9A2 H 0.617454 0.360827 0.837997 0.102 Uiso 0.678(9) 1 calc R U P A 1
H9A3 H 0.633803 0.432771 0.933505 0.102 Uiso 0.678(9) 1 calc R U P A 1
C10A C 0.7783(7) 0.6714(7) 0.8895(4) 0.0397(19) Uiso 0.678(9) 1 d . . P A 1
H10A H 0.865478 0.663079 0.893605 0.060 Uiso 0.678(9) 1 calc R U P A 1
H10B H 0.748258 0.672697 0.948804 0.060 Uiso 0.678(9) 1 calc R U P A 1
H10C H 0.784207 0.751488 0.862497 0.060 Uiso 0.678(9) 1 calc R U P A 1
C8B C 0.7494(15) 0.5581(13) 0.8420(9) 0.030(3) Uiso 0.322(9) 1 d . . P A 2
H8B H 0.838945 0.622039 0.861726 0.036 Uiso 0.322(9) 1 calc R U P A 2
C9B C 0.7356(13) 0.4237(12) 0.8752(9) 0.026(3) Uiso 0.322(9) 1 d . . P A 2
H9B1 H 0.739802 0.427821 0.939821 0.039 Uiso 0.322(9) 1 calc R U P A 2
H9B2 H 0.807786 0.398405 0.855411 0.039 Uiso 0.322(9) 1 calc R U P A 2
H9B3 H 0.650678 0.360306 0.851061 0.039 Uiso 0.322(9) 1 calc R U P A 2
C10B C 0.6454(14) 0.6021(14) 0.8739(10) 0.039(4) Uiso 0.322(9) 1 d . . P A 2
H10D H 0.643458 0.676292 0.842056 0.059 Uiso 0.322(9) 1 calc R U P A 2
H10E H 0.664476 0.626622 0.937280 0.059 Uiso 0.322(9) 1 calc R U P A 2
H10F H 0.559348 0.532471 0.863480 0.059 Uiso 0.322(9) 1 calc R U P A 2
C11 C 0.5413(4) 0.7678(4) 0.6961(3) 0.0302(9) Uani 1 1 d . . . . .
H11 H 0.483096 0.692754 0.663260 0.036 Uiso 1 1 calc R U . . .
C12 C 0.4891(4) 0.8440(4) 0.7432(3) 0.0350(10) Uani 1 1 d . . . . .
H12 H 0.396080 0.821621 0.742767 0.042 Uiso 1 1 calc R U . . .
C13 C 0.5724(4) 0.9523(4) 0.7907(3) 0.0359(10) Uani 1 1 d . . . . .
H13 H 0.537709 1.004121 0.825013 0.043 Uiso 1 1 calc R U . . .
C14 C 0.7078(4) 0.9852(4) 0.7882(3) 0.0306(9) Uani 1 1 d . . . . .
H14 H 0.767124 1.060583 0.820077 0.037 Uiso 1 1 calc R U . . .
C15 C 0.7552(4) 0.9072(4) 0.7388(2) 0.0244(8) Uani 1 1 d . . . . .
C16 C 0.9002(4) 0.9364(4) 0.7321(3) 0.0264(8) Uani 1 1 d . . . . .
H16A H 0.944402 1.028494 0.722432 0.032 Uiso 1 1 calc R U . . .
H16B H 0.940766 0.917768 0.787753 0.032 Uiso 1 1 calc R U . . .
C17 C 1.0187(3) 0.9032(3) 0.6119(2) 0.0194(7) Uani 1 1 d . . . . .
C18 C 1.1300(3) 0.8381(3) 0.4905(2) 0.0205(7) Uani 1 1 d . . . . .
C19 C 1.1110(4) 0.7982(4) 0.4014(2) 0.0234(8) Uani 1 1 d . . . . .
H19 H 1.026011 0.777127 0.370918 0.028 Uiso 1 1 calc R U . . .
C20 C 1.2150(4) 0.7889(4) 0.3566(2) 0.0244(8) Uani 1 1 d . . . . .
H20 H 1.199391 0.758416 0.296170 0.029 Uiso 1 1 calc R U . . .
C21 C 1.3419(4) 0.8233(3) 0.3985(2) 0.0221(8) Uani 1 1 d . . . . .
C22 C 1.3582(4) 0.8579(4) 0.4888(3) 0.0241(8) Uani 1 1 d . . . . .
H22 H 1.442977 0.878258 0.519531 0.029 Uiso 1 1 calc R U . . .
C23 C 1.2540(3) 0.8634(3) 0.5349(2) 0.0218(7) Uani 1 1 d . . . . .
H23 H 1.267094 0.884535 0.596779 0.026 Uiso 1 1 calc R U . . .
C24 C 1.4577(4) 0.8246(4) 0.3483(3) 0.0259(8) Uani 1 1 d . . . . .
H24A H 1.425365 0.780950 0.289660 0.039 Uiso 1 1 calc R U . . .
H24B H 1.508143 0.780010 0.380602 0.039 Uiso 1 1 calc R U . . .
H24C H 1.514852 0.913532 0.342021 0.039 Uiso 1 1 calc R U . . .
C25 C 1.1907(3) 1.0415(4) 0.7234(2) 0.0224(8) Uani 1 1 d . . . . .
C26 C 1.2558(4) 1.1693(4) 0.7535(3) 0.0288(9) Uani 1 1 d . . . . .
H26 H 1.252076 1.236626 0.718087 0.035 Uiso 1 1 calc R U . . .
C27 C 1.3264(4) 1.1971(4) 0.8360(3) 0.0360(10) Uani 1 1 d . . . . .
H27 H 1.371557 1.284290 0.856202 0.043 Uiso 1 1 calc R U . . .
C28 C 1.3330(4) 1.1019(5) 0.8895(3) 0.0364(10) Uani 1 1 d . . . . .
C29 C 1.2655(4) 0.9731(4) 0.8582(3) 0.0306(9) Uani 1 1 d . . . . .
H29 H 1.267696 0.905702 0.894000 0.037 Uiso 1 1 calc R U . . .
C30 C 1.1963(4) 0.9442(4) 0.7759(3) 0.0266(8) Uani 1 1 d . . . . .
H30 H 1.152206 0.857022 0.755162 0.032 Uiso 1 1 calc R U . . .
C31 C 1.4087(5) 1.1331(6) 0.9800(3) 0.0554(14) Uani 1 1 d . . . . .
H31A H 1.495708 1.125952 0.976087 0.083 Uiso 1 1 calc R U . . .
H31B H 1.359437 1.072776 1.021439 0.083 Uiso 1 1 calc R U . . .
H31C H 1.419786 1.220895 1.000820 0.083 Uiso 1 1 calc R U . . .
Sb Sb 0.79974(2) 0.47204(3) 0.18081(2) 0.02611(7) Uani 1 1 d . . . . .
F1 F 0.6700(3) 0.3349(3) 0.11622(17) 0.0500(7) Uani 1 1 d . . . . .
F2 F 0.9297(3) 0.6095(3) 0.24594(17) 0.0506(7) Uani 1 1 d . . . . .
F3 F 0.8162(3) 0.3621(2) 0.26819(16) 0.0409(6) Uani 1 1 d . . . . .
F4 F 0.7847(3) 0.5836(3) 0.09549(17) 0.0420(6) Uani 1 1 d . . . . .
F5 F 0.9305(3) 0.4368(3) 0.12192(18) 0.0560(8) Uani 1 1 d . . . . .
F6 F 0.6699(2) 0.5055(2) 0.24244(17) 0.0405(6) Uani 1 1 d . . . . .
H3N H 0.942(2) 0.804(3) 0.506(2) 0.022(10) Uiso 1 1 d D . . . .
H4N H 1.162(3) 1.047(3) 0.5933(18) 0.016(10) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os N1 2.092(3) . ?
Os N2 2.106(3) . ?
Os C3 2.164(4) . ?
Os C2 2.187(4) . ?
Os C5 2.190(4) . ?
Os C6 2.192(4) . ?
Os C4 2.204(4) . ?
Os C1 2.213(4) . ?
Os Cl 2.4230(9) . ?
N1 C15 1.349(5) . ?
N1 C11 1.351(5) . ?
N2 C17 1.302(4) . ?
N2 C16 1.469(5) . ?
N3 C17 1.362(4) . ?
N3 C18 1.411(4) . ?
N3 H3N 0.863(18) . ?
N4 C17 1.371(5) . ?
N4 C25 1.424(5) . ?
N4 H4N 0.846(18) . ?
C1 C2 1.392(6) . ?
C1 C6 1.438(5) . ?
C1 C7 1.499(6) . ?
C2 C3 1.416(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.408(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.424(6) . ?
C4 C8B 1.537(13) . ?
C4 C8A 1.555(8) . ?
C5 C6 1.396(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8A C10A 1.506(10) . ?
C8A C9A 1.535(11) . ?
C8A H8A 1.0000 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C8B C10B 1.48(2) . ?
C8B C9B 1.560(18) . ?
C8B H8B 1.0000 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11 C12 1.378(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.369(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.387(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.501(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 C19 1.388(5) . ?
C18 C23 1.393(5) . ?
C19 C20 1.388(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.393(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.394(5) . ?
C21 C24 1.509(5) . ?
C22 C23 1.387(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C30 1.388(5) . ?
C25 C26 1.392(5) . ?
C26 C27 1.391(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.379(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.410(6) . ?
C28 C31 1.516(6) . ?
C29 C30 1.381(5) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
Sb F1 1.864(2) . ?
Sb F4 1.869(2) . ?
Sb F2 1.870(2) . ?
Sb F5 1.870(3) . ?
Sb F6 1.875(2) . ?
Sb F3 1.883(2) . ?

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 Os N2 76.58(12) . . ?
N1 Os C3 119.41(15) . . ?
N2 Os C3 93.79(14) . . ?
N1 Os C2 156.81(15) . . ?
N2 Os C2 96.92(14) . . ?
C3 Os C2 37.97(16) . . ?
N1 Os C5 96.30(14) . . ?
N2 Os C5 154.09(14) . . ?
C3 Os C5 67.71(16) . . ?
C2 Os C5 79.78(15) . . ?
N1 Os C6 122.08(14) . . ?
N2 Os C6 161.08(13) . . ?
C3 Os C6 79.90(15) . . ?
C2 Os C6 67.16(15) . . ?
C5 Os C6 37.16(15) . . ?
N1 Os C4 94.68(15) . . ?
N2 Os C4 117.05(14) . . ?
C3 Os C4 37.60(17) . . ?
C2 Os C4 68.15(17) . . ?
C5 Os C4 37.82(16) . . ?
C6 Os C4 67.81(15) . . ?
N1 Os C1 159.77(14) . . ?
N2 Os C1 123.02(13) . . ?
C3 Os C1 68.01(16) . . ?
C2 Os C1 36.89(16) . . ?
C5 Os C1 68.21(15) . . ?
C6 Os C1 38.11(14) . . ?
C4 Os C1 81.03(15) . . ?
N1 Os Cl 84.02(9) . . ?
N2 Os Cl 86.29(8) . . ?
C3 Os Cl 155.97(13) . . ?
C2 Os Cl 118.12(12) . . ?
C5 Os Cl 118.11(12) . . ?
C6 Os Cl 92.33(10) . . ?
C4 Os Cl 155.75(12) . . ?
C1 Os Cl 91.84(11) . . ?
C15 N1 C11 118.9(3) . . ?
C15 N1 Os 117.1(2) . . ?
C11 N1 Os 124.0(3) . . ?
C17 N2 C16 119.2(3) . . ?
C17 N2 Os 127.4(2) . . ?
C16 N2 Os 113.3(2) . . ?
C17 N3 C18 127.8(3) . . ?
C17 N3 H3N 114(3) . . ?
C18 N3 H3N 118(3) . . ?
C17 N4 C25 124.1(3) . . ?
C17 N4 H4N 111(3) . . ?
C25 N4 H4N 120(3) . . ?
C2 C1 C6 117.6(4) . . ?
C2 C1 C7 121.6(4) . . ?
C6 C1 C7 120.7(4) . . ?
C2 C1 Os 70.5(2) . . ?
C6 C1 Os 70.1(2) . . ?
C7 C1 Os 128.9(3) . . ?
C1 C2 C3 121.3(4) . . ?
C1 C2 Os 72.6(2) . . ?
C3 C2 Os 70.1(2) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
Os C2 H2 130.8 . . ?
C4 C3 C2 121.2(4) . . ?
C4 C3 Os 72.7(2) . . ?
C2 C3 Os 71.9(2) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
Os C3 H3 128.2 . . ?
C3 C4 C5 117.8(4) . . ?
C3 C4 C8B 102.9(6) . . ?
C5 C4 C8B 138.6(7) . . ?
C3 C4 C8A 129.2(5) . . ?
C5 C4 C8A 112.9(5) . . ?
C3 C4 Os 69.7(2) . . ?
C5 C4 Os 70.5(2) . . ?
C8B C4 Os 135.7(6) . . ?
C8A C4 Os 128.6(4) . . ?
C6 C5 C4 120.8(4) . . ?
C6 C5 Os 71.5(2) . . ?
C4 C5 Os 71.6(2) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
Os C5 H5 129.8 . . ?
C5 C6 C1 121.2(4) . . ?
C5 C6 Os 71.3(2) . . ?
C1 C6 Os 71.7(2) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
Os C6 H6 130.1 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10A C8A C9A 108.8(7) . . ?
C10A C8A C4 112.2(6) . . ?
C9A C8A C4 105.2(6) . . ?
C10A C8A H8A 110.2 . . ?
C9A C8A H8A 110.2 . . ?
C4 C8A H8A 110.2 . . ?
C8A C9A H9A1 109.5 . . ?
C8A C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C8A C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C8A C10A H10A 109.5 . . ?
C8A C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C8A C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C10B C8B C4 106.7(11) . . ?
C10B C8B C9B 111.0(11) . . ?
C4 C8B C9B 108.3(9) . . ?
C10B C8B H8B 110.2 . . ?
C4 C8B H8B 110.2 . . ?
C9B C8B H8B 110.2 . . ?
C8B C9B H9B1 109.5 . . ?
C8B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C8B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C8B C10B H10D 109.5 . . ?
C8B C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C8B C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
N1 C11 C12 121.5(4) . . ?
N1 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C13 C12 C11 119.6(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C15 C14 C13 119.1(4) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N1 C15 C14 121.6(4) . . ?
N1 C15 C16 116.0(3) . . ?
C14 C15 C16 122.4(4) . . ?
N2 C16 C15 108.9(3) . . ?
N2 C16 H16A 109.9 . . ?
C15 C16 H16A 109.9 . . ?
N2 C16 H16B 109.9 . . ?
C15 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
N2 C17 N3 119.5(3) . . ?
N2 C17 N4 123.0(3) . . ?
N3 C17 N4 117.4(3) . . ?
C19 C18 C23 118.8(3) . . ?
C19 C18 N3 117.5(3) . . ?
C23 C18 N3 123.7(3) . . ?
C18 C19 C20 120.6(3) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C19 C20 C21 121.2(3) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C20 C21 C22 117.5(3) . . ?
C20 C21 C24 121.4(3) . . ?
C22 C21 C24 121.1(3) . . ?
C23 C22 C21 121.7(3) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C22 C23 C18 120.0(3) . . ?
C22 C23 H23 120.0 . . ?
C18 C23 H23 120.0 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 119.9(4) . . ?
C30 C25 N4 121.5(3) . . ?
C26 C25 N4 118.5(3) . . ?
C27 C26 C25 119.0(4) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C28 C27 C26 122.1(4) . . ?
C28 C27 H27 119.0 . . ?
C26 C27 H27 119.0 . . ?
C27 C28 C29 118.0(4) . . ?
C27 C28 C31 121.7(4) . . ?
C29 C28 C31 120.3(4) . . ?
C30 C29 C28 120.5(4) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C25 120.4(4) . . ?
C29 C30 H30 119.8 . . ?
C25 C30 H30 119.8 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
F1 Sb F4 90.50(12) . . ?
F1 Sb F2 179.84(14) . . ?
F4 Sb F2 89.63(12) . . ?
F1 Sb F5 90.09(14) . . ?
F4 Sb F5 91.05(12) . . ?
F2 Sb F5 90.00(13) . . ?
F1 Sb F6 90.29(12) . . ?
F4 Sb F6 90.39(11) . . ?
F2 Sb F6 89.61(12) . . ?
F5 Sb F6 178.51(12) . . ?
F1 Sb F3 90.41(12) . . ?
F4 Sb F3 179.02(11) . . ?
F2 Sb F3 89.45(12) . . ?
F5 Sb F3 89.31(12) . . ?
F6 Sb F3 89.25(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -1.2(6) . . . . ?
C7 C1 C2 C3 176.9(4) . . . . ?
Os C1 C2 C3 52.5(4) . . . . ?
C6 C1 C2 Os -53.7(3) . . . . ?
C7 C1 C2 Os 124.4(4) . . . . ?
C1 C2 C3 C4 2.1(6) . . . . ?
Os C2 C3 C4 55.8(4) . . . . ?
C1 C2 C3 Os -53.6(4) . . . . ?
C2 C3 C4 C5 -2.1(6) . . . . ?
Os C3 C4 C5 53.3(3) . . . . ?
C2 C3 C4 C8B 170.4(6) . . . . ?
Os C3 C4 C8B -134.3(6) . . . . ?
C2 C3 C4 C8A -179.1(5) . . . . ?
Os C3 C4 C8A -123.8(5) . . . . ?
C2 C3 C4 Os -55.4(4) . . . . ?
C3 C4 C5 C6 1.1(6) . . . . ?
C8B C4 C5 C6 -167.6(9) . . . . ?
C8A C4 C5 C6 178.7(4) . . . . ?
Os C4 C5 C6 54.0(3) . . . . ?
C3 C4 C5 Os -52.9(3) . . . . ?
C8B C4 C5 Os 138.3(9) . . . . ?
C8A C4 C5 Os 124.7(4) . . . . ?
C4 C5 C6 C1 -0.3(6) . . . . ?
Os C5 C6 C1 53.8(3) . . . . ?
C4 C5 C6 Os -54.1(3) . . . . ?
C2 C1 C6 C5 0.3(6) . . . . ?
C7 C1 C6 C5 -177.9(4) . . . . ?
Os C1 C6 C5 -53.6(3) . . . . ?
C2 C1 C6 Os 53.9(3) . . . . ?
C7 C1 C6 Os -124.2(4) . . . . ?
C3 C4 C8A C10A 30.6(8) . . . . ?
C5 C4 C8A C10A -146.6(5) . . . . ?
Os C4 C8A C10A -63.8(8) . . . . ?
C3 C4 C8A C9A -87.5(7) . . . . ?
C5 C4 C8A C9A 95.3(6) . . . . ?
Os C4 C8A C9A 178.1(5) . . . . ?
C3 C4 C8B C10B 147.1(9) . . . . ?
C5 C4 C8B C10B -43.1(14) . . . . ?
Os C4 C8B C10B 73.1(13) . . . . ?
C3 C4 C8B C9B -93.3(9) . . . . ?
C5 C4 C8B C9B 76.5(13) . . . . ?
Os C4 C8B C9B -167.3(6) . . . . ?
C15 N1 C11 C12 -3.2(6) . . . . ?
Os N1 C11 C12 174.8(3) . . . . ?
N1 C11 C12 C13 0.0(6) . . . . ?
C11 C12 C13 C14 2.0(6) . . . . ?
C12 C13 C14 C15 -0.8(6) . . . . ?
C11 N1 C15 C14 4.4(5) . . . . ?
Os N1 C15 C14 -173.7(3) . . . . ?
C11 N1 C15 C16 -177.5(3) . . . . ?
Os N1 C15 C16 4.3(4) . . . . ?
C13 C14 C15 N1 -2.5(6) . . . . ?
C13 C14 C15 C16 179.6(4) . . . . ?
C17 N2 C16 C15 146.0(3) . . . . ?
Os N2 C16 C15 -30.1(4) . . . . ?
N1 C15 C16 N2 16.9(5) . . . . ?
C14 C15 C16 N2 -165.1(3) . . . . ?
C16 N2 C17 N3 -164.4(3) . . . . ?
Os N2 C17 N3 11.1(5) . . . . ?
C16 N2 C17 N4 11.1(5) . . . . ?
Os N2 C17 N4 -173.3(3) . . . . ?
C18 N3 C17 N2 -149.1(4) . . . . ?
C18 N3 C17 N4 35.0(5) . . . . ?
C25 N4 C17 N2 49.3(5) . . . . ?
C25 N4 C17 N3 -135.0(4) . . . . ?
C17 N3 C18 C19 -166.3(4) . . . . ?
C17 N3 C18 C23 16.6(6) . . . . ?
C23 C18 C19 C20 -2.6(6) . . . . ?
N3 C18 C19 C20 -179.8(3) . . . . ?
C18 C19 C20 C21 -2.3(6) . . . . ?
C19 C20 C21 C22 4.9(6) . . . . ?
C19 C20 C21 C24 -174.5(3) . . . . ?
C20 C21 C22 C23 -2.7(6) . . . . ?
C24 C21 C22 C23 176.7(3) . . . . ?
C21 C22 C23 C18 -2.1(6) . . . . ?
C19 C18 C23 C22 4.7(5) . . . . ?
N3 C18 C23 C22 -178.2(3) . . . . ?
C17 N4 C25 C30 26.6(5) . . . . ?
C17 N4 C25 C26 -155.2(3) . . . . ?
C30 C25 C26 C27 0.4(6) . . . . ?
N4 C25 C26 C27 -177.8(3) . . . . ?
C25 C26 C27 C28 -0.6(6) . . . . ?
C26 C27 C28 C29 0.1(6) . . . . ?
C26 C27 C28 C31 -179.1(4) . . . . ?
C27 C28 C29 C30 0.6(6) . . . . ?
C31 C28 C29 C30 179.9(4) . . . . ?
C28 C29 C30 C25 -0.9(6) . . . . ?
C26 C25 C30 C29 0.4(6) . . . . ?
N4 C25 C30 C29 178.5(3) . . . . ?

_refine_diff_density_max         1.322
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.115


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/methanol'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cmpnd_6
_database_code_depnum_ccdc_archive 'CCDC 1983334'
loop_
_audit_author_name
_audit_author_address
'Pilar Garcia-Orduna'
;Instituto de Sintesis Quimica y Catalisis Homogenea (ISQCH, CSIC Univ Zaragoza)
Spain
;
_audit_update_record             
;
2020-07-31 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H41 N5 Os, 2(F6 Sb)'
_chemical_formula_sum            'C36 H41 F12 N5 Os Sb2'
_chemical_formula_weight         1205.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5507(13)
_cell_length_b                   11.8469(13)
_cell_length_c                   15.5684(17)
_cell_angle_alpha                72.5690(10)
_cell_angle_beta                 80.2290(10)
_cell_angle_gamma                82.140(2)
_cell_volume                     1994.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5038
_cell_measurement_theta_min      2.393
_cell_measurement_theta_max      27.968

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_F_000             1156
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    4.612
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5482
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_process_details   'twinabs 2008/2'


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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 APEX CCD system'
_diffrn_measurement_method       'narrow ω frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            19485
_diffrn_reflns_av_unetI/netI     0.1035
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.796
_diffrn_reflns_theta_max         28.288
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13387
_reflns_number_gt                9481
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_cell_refinement       'CELL_NOW (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'

_refine_special_details          
;Refined as a 2-component twin related by a 180 degres rotation around
reciprocal b axis. TWINABS data correction indicates the presence of:
6813 data (3664 unique) involving only domain 1. mean I/sigma= 5.7
6761 data (3634 unique) involving only domain 2. mean I/sigma= 3.1
10816 data (6115 unique) involve both domains. mean I/sigma= 4.9
Then, both domain contributions have been included in the integration
and the absorption corrections. Final structural model refinement
leads to a 0.289 BASF value.

The asymmetric unit contains an Osmium complex and two SbF6 counterions.
Most of the hydrogen atoms have been included in the model in calculated
positions and refined with a riding model. Hydrogen atoms of NH fragments
have been included in observed positions. Their free refinement leads
to a too short N4-H4N distance and a too small Uiso(H3N). Therefore, 
appropiate restraints have been used.

At the end of the refinement, when convergence is achieved, highest
residual density peaks are observed close to Osmium atom. They have no
chemical sense.,Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0516P)²+10.8388P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Direct method'
_atom_sites_solution_secondary   'Fourier Difference Synthesis'
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13387
_refine_ls_number_parameters     518
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_ref         0.1352
_refine_ls_wR_factor_gt          0.1153
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.64608(4) 0.80641(4) 0.35045(3) 0.01454(11) Uani 1 1 d . . . . .
N1 N 0.6625(8) 0.6472(8) 0.3141(6) 0.018(2) Uani 1 1 d . . . . .
N2 N 0.5165(7) 0.8394(8) 0.2624(6) 0.016(2) Uani 1 1 d . . . . .
N3 N 0.4664(9) 1.0383(8) 0.2511(7) 0.018(2) Uani 1 1 d . . . . .
H3N H 0.543(11) 1.043(10) 0.238(8) 0.021 Uiso 1 1 d . U . . .
N4 N 0.3464(8) 0.9353(9) 0.1998(7) 0.019(2) Uani 1 1 d D . . . .
N5 N 0.7740(8) 0.8440(8) 0.2309(6) 0.017(2) Uani 1 1 d . . . . .
C1 C 0.5681(11) 0.7432(11) 0.4961(8) 0.022(3) Uani 1 1 d . . . . .
C2 C 0.6951(10) 0.7180(11) 0.4867(7) 0.017(2) Uani 1 1 d . . . . .
H2 H 0.7288 0.6391 0.5099 0.021 Uiso 1 1 calc R U . . .
C3 C 0.7684(9) 0.8089(10) 0.4437(7) 0.013(2) Uani 1 1 d . . . . .
H3 H 0.8515 0.7906 0.4390 0.015 Uiso 1 1 calc R U . . .
C4 C 0.7223(9) 0.9272(9) 0.4072(7) 0.013(2) Uani 1 1 d . . . . .
C5 C 0.5992(10) 0.9545(11) 0.4147(8) 0.022(3) Uani 1 1 d . . . . .
H5 H 0.5667 1.0340 0.3915 0.026 Uiso 1 1 calc R U . . .
C6 C 0.5222(10) 0.8600(10) 0.4582(7) 0.017(2) Uani 1 1 d . . . . .
H6 H 0.4391 0.8780 0.4610 0.020 Uiso 1 1 calc R U . . .
C7 C 0.4906(11) 0.6458(11) 0.5437(8) 0.027(3) Uani 1 1 d . . . . .
H7A H 0.5270 0.5717 0.5311 0.040 Uiso 1 1 calc R U . . .
H7B H 0.4135 0.6663 0.5220 0.040 Uiso 1 1 calc R U . . .
H7C H 0.4804 0.6355 0.6093 0.040 Uiso 1 1 calc R U . . .
C8 C 0.8070(10) 1.0214(10) 0.3586(8) 0.021(3) Uani 1 1 d . . . . .
H8 H 0.8741 0.9833 0.3241 0.025 Uiso 1 1 calc R U . . .
C9 C 0.7557(11) 1.1309(12) 0.2908(9) 0.034(3) Uani 1 1 d . . . . .
H9A H 0.7191 1.1059 0.2479 0.051 Uiso 1 1 calc R U . . .
H9B H 0.8189 1.1810 0.2575 0.051 Uiso 1 1 calc R U . . .
H9C H 0.6962 1.1760 0.3235 0.051 Uiso 1 1 calc R U . . .
C10 C 0.8576(11) 1.0574(13) 0.4297(9) 0.032(3) Uani 1 1 d . . . . .
H10A H 0.9231 1.1061 0.4001 0.049 Uiso 1 1 calc R U . . .
H10B H 0.8862 0.9860 0.4746 0.049 Uiso 1 1 calc R U . . .
H10C H 0.7959 1.1031 0.4602 0.049 Uiso 1 1 calc R U . . .
C11 C 0.7489(10) 0.5588(10) 0.3377(7) 0.018(2) Uani 1 1 d . . . . .
H11 H 0.7947 0.5609 0.3824 0.022 Uiso 1 1 calc R U . . .
C12 C 0.7729(10) 0.4656(11) 0.2993(8) 0.025(3) Uani 1 1 d . . . . .
H12 H 0.8339 0.4047 0.3173 0.030 Uiso 1 1 calc R U . . .
C13 C 0.7060(10) 0.4624(11) 0.2333(7) 0.021(3) Uani 1 1 d . . . . .
H13 H 0.7224 0.4006 0.2046 0.025 Uiso 1 1 calc R U . . .
C14 C 0.6148(11) 0.5512(10) 0.2103(8) 0.021(3) Uani 1 1 d . . . . .
H14 H 0.5661 0.5498 0.1672 0.026 Uiso 1 1 calc R U . . .
C15 C 0.5972(10) 0.6409(10) 0.2516(7) 0.017(2) Uani 1 1 d . . . . .
C16 C 0.4986(11) 0.7378(10) 0.2325(8) 0.022(3) Uani 1 1 d . . . . .
H16A H 0.4938 0.7643 0.1665 0.026 Uiso 1 1 calc R U . . .
H16B H 0.4230 0.7063 0.2643 0.026 Uiso 1 1 calc R U . . .
C17 C 0.4433(10) 0.9359(10) 0.2387(7) 0.019(2) Uani 1 1 d . . . . .
C18 C 0.3876(11) 1.1338(11) 0.2705(8) 0.021(3) Uani 1 1 d . . . . .
C19 C 0.2792(10) 1.1104(11) 0.3237(7) 0.020(3) Uani 1 1 d . . . . .
H19 H 0.2600 1.0308 0.3506 0.024 Uiso 1 1 calc R U . . .
C20 C 0.1998(11) 1.2038(11) 0.3371(8) 0.026(3) Uani 1 1 d . . . . .
H20 H 0.1248 1.1877 0.3718 0.032 Uiso 1 1 calc R U . . .
C21 C 0.2274(11) 1.3216(11) 0.3007(8) 0.025(3) Uani 1 1 d . . . . .
C22 C 0.3396(11) 1.3409(12) 0.2526(9) 0.029(3) Uani 1 1 d . . . . .
H22 H 0.3625 1.4196 0.2301 0.035 Uiso 1 1 calc R U . . .
C23 C 0.4182(12) 1.2481(11) 0.2371(9) 0.027(3) Uani 1 1 d . . . . .
H23 H 0.4937 1.2635 0.2030 0.033 Uiso 1 1 calc R U . . .
C24 C 0.1390(12) 1.4226(12) 0.3097(9) 0.034(3) Uani 1 1 d . . . . .
H24A H 0.0894 1.4003 0.3688 0.051 Uiso 1 1 calc R U . . .
H24B H 0.0895 1.4423 0.2610 0.051 Uiso 1 1 calc R U . . .
H24C H 0.1798 1.4918 0.3053 0.051 Uiso 1 1 calc R U . . .
C25 C 0.2822(10) 1.0397(10) 0.1492(8) 0.018(2) Uani 1 1 d . . . . .
C26 C 0.1606(10) 1.0530(11) 0.1671(8) 0.021(3) Uani 1 1 d . . . . .
H26 H 0.1189 0.9911 0.2094 0.025 Uiso 1 1 calc R U . . .
C27 C 0.1001(11) 1.1578(11) 0.1226(8) 0.025(3) Uani 1 1 d . . . . .
H27 H 0.0164 1.1662 0.1346 0.030 Uiso 1 1 calc R U . . .
C28 C 0.1570(12) 1.2498(12) 0.0619(9) 0.031(3) Uani 1 1 d . . . . .
C29 C 0.2815(12) 1.2335(12) 0.0410(9) 0.032(3) Uani 1 1 d . . . . .
H29 H 0.3230 1.2950 -0.0019 0.038 Uiso 1 1 calc R U . . .
C30 C 0.3424(11) 1.1275(11) 0.0833(8) 0.024(3) Uani 1 1 d . . . . .
H30 H 0.4252 1.1148 0.0671 0.029 Uiso 1 1 calc R U . . .
C31 C 0.0936(14) 1.3657(13) 0.0145(11) 0.050(4) Uani 1 1 d . . . . .
H31A H 0.1341 1.4318 0.0172 0.076 Uiso 1 1 calc R U . . .
H31B H 0.0122 1.3717 0.0446 0.076 Uiso 1 1 calc R U . . .
H31C H 0.0933 1.3692 -0.0491 0.076 Uiso 1 1 calc R U . . .
C32 C 0.7493(10) 0.9145(10) 0.1491(7) 0.020(3) Uani 1 1 d . . . . .
H32 H 0.6721 0.9532 0.1438 0.023 Uiso 1 1 calc R U . . .
C33 C 0.8332(11) 0.9319(12) 0.0727(8) 0.025(3) Uani 1 1 d . . . . .
H33 H 0.8137 0.9824 0.0160 0.030 Uiso 1 1 calc R U . . .
C34 C 0.9460(11) 0.8752(12) 0.0794(8) 0.028(3) Uani 1 1 d . . . . .
H34 H 1.0042 0.8847 0.0274 0.033 Uiso 1 1 calc R U . . .
C35 C 0.9721(10) 0.8045(12) 0.1637(8) 0.027(3) Uani 1 1 d . . . . .
H35 H 1.0492 0.7661 0.1704 0.032 Uiso 1 1 calc R U . . .
C36 C 0.8850(10) 0.7901(10) 0.2380(8) 0.020(2) Uani 1 1 d . . . . .
H36 H 0.9033 0.7412 0.2955 0.024 Uiso 1 1 calc R U . . .
Sb1 Sb 0.69892(7) 0.29415(8) -0.00778(5) 0.0228(2) Uani 1 1 d . . . . .
F1 F 0.6222(7) 0.1702(7) 0.0787(5) 0.041(2) Uani 1 1 d . . . . .
F2 F 0.7806(8) 0.4126(8) -0.0931(6) 0.059(3) Uani 1 1 d . . . . .
F3 F 0.7462(7) 0.1916(7) -0.0813(5) 0.044(2) Uani 1 1 d . . . . .
F4 F 0.6498(8) 0.3922(8) 0.0683(6) 0.053(2) Uani 1 1 d . . . . .
F5 F 0.8340(7) 0.2363(8) 0.0492(6) 0.052(2) Uani 1 1 d . . . . .
F6 F 0.5628(7) 0.3446(8) -0.0626(6) 0.052(2) Uani 1 1 d . . . . .
Sb2 Sb 0.15037(7) 0.70944(7) 0.41317(5) 0.01802(18) Uani 1 1 d . . . . .
F7 F 0.1040(6) 0.6975(7) 0.5371(4) 0.0340(18) Uani 1 1 d . . . . .
F8 F 0.1997(6) 0.7229(6) 0.2894(4) 0.0287(17) Uani 1 1 d . . . . .
F9 F 0.2457(6) 0.5657(6) 0.4443(5) 0.0314(18) Uani 1 1 d . . . . .
F10 F 0.0589(6) 0.8550(6) 0.3814(5) 0.0332(18) Uani 1 1 d . . . . .
F11 F 0.0211(6) 0.6297(6) 0.4123(5) 0.0315(17) Uani 1 1 d . . . . .
F12 F 0.2792(6) 0.7913(6) 0.4127(4) 0.0263(16) Uani 1 1 d . . . . .
H4N H 0.317(10) 0.870(6) 0.204(9) 0.03(4) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os N1 2.102(9) . ?
Os N2 2.118(9) . ?
Os N5 2.144(9) . ?
Os C2 2.198(10) . ?
Os C3 2.199(10) . ?
Os C6 2.200(11) . ?
Os C4 2.229(10) . ?
Os C5 2.232(11) . ?
Os C1 2.233(11) . ?
N1 C15 1.352(14) . ?
N1 C11 1.355(13) . ?
N2 C17 1.321(14) . ?
N2 C16 1.464(14) . ?
N3 C17 1.352(14) . ?
N3 C18 1.425(14) . ?
N3 H3N 0.87(12) . ?
N4 C17 1.363(14) . ?
N4 C25 1.437(14) . ?
N4 H4N 0.87(2) . ?
N5 C32 1.350(13) . ?
N5 C36 1.358(14) . ?
C1 C6 1.400(15) . ?
C1 C2 1.448(16) . ?
C1 C7 1.492(16) . ?
C2 C3 1.396(15) . ?
C2 H2 0.9500 . ?
C3 C4 1.411(15) . ?
C3 H3 0.9500 . ?
C4 C5 1.407(15) . ?
C4 C8 1.522(15) . ?
C5 C6 1.456(16) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.522(15) . ?
C8 C9 1.527(17) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.383(15) . ?
C11 H11 0.9500 . ?
C12 C13 1.397(15) . ?
C12 H12 0.9500 . ?
C13 C14 1.394(16) . ?
C13 H13 0.9500 . ?
C14 C15 1.375(15) . ?
C14 H14 0.9500 . ?
C15 C16 1.502(15) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 C23 1.369(17) . ?
C18 C19 1.391(16) . ?
C19 C20 1.380(15) . ?
C19 H19 0.9500 . ?
C20 C21 1.399(17) . ?
C20 H20 0.9500 . ?
C21 C22 1.394(17) . ?
C21 C24 1.487(16) . ?
C22 C23 1.380(17) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.382(15) . ?
C25 C30 1.390(16) . ?
C26 C27 1.386(16) . ?
C26 H26 0.9500 . ?
C27 C28 1.371(18) . ?
C27 H27 0.9500 . ?
C28 C29 1.419(18) . ?
C28 C31 1.506(18) . ?
C29 C30 1.388(17) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.383(15) . ?
C32 H32 0.9500 . ?
C33 C34 1.388(17) . ?
C33 H33 0.9500 . ?
C34 C35 1.386(17) . ?
C34 H34 0.9500 . ?
C35 C36 1.382(15) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
Sb1 F2 1.855(8) . ?
Sb1 F6 1.858(8) . ?
Sb1 F4 1.869(8) . ?
Sb1 F5 1.871(8) . ?
Sb1 F1 1.876(7) . ?
Sb1 F3 1.877(7) . ?
Sb2 F10 1.871(7) . ?
Sb2 F11 1.876(7) . ?
Sb2 F9 1.877(7) . ?
Sb2 F8 1.878(6) . ?
Sb2 F7 1.880(7) . ?
Sb2 F12 1.881(6) . ?

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 Os N2 77.6(3) . . ?
N1 Os N5 78.5(3) . . ?
N2 Os N5 87.1(3) . . ?
N1 Os C2 93.7(4) . . ?
N2 Os C2 147.2(4) . . ?
N5 Os C2 122.6(4) . . ?
N1 Os C3 114.1(4) . . ?
N2 Os C3 168.3(4) . . ?
N5 Os C3 95.1(4) . . ?
C2 Os C3 37.0(4) . . ?
N1 Os C6 128.8(4) . . ?
N2 Os C6 93.4(4) . . ?
N5 Os C6 152.2(4) . . ?
C2 Os C6 67.4(4) . . ?
C3 Os C6 79.4(4) . . ?
N1 Os C4 149.1(4) . . ?
N2 Os C4 131.5(4) . . ?
N5 Os C4 91.2(4) . . ?
C2 Os C4 67.3(4) . . ?
C3 Os C4 37.2(4) . . ?
C6 Os C4 67.8(4) . . ?
N1 Os C5 167.0(4) . . ?
N2 Os C5 102.1(4) . . ?
N5 Os C5 114.5(4) . . ?
C2 Os C5 79.5(4) . . ?
C3 Os C5 66.5(4) . . ?
C6 Os C5 38.3(4) . . ?
C4 Os C5 36.8(4) . . ?
N1 Os C1 100.1(4) . . ?
N2 Os C1 111.6(4) . . ?
N5 Os C1 160.7(4) . . ?
C2 Os C1 38.1(4) . . ?
C3 Os C1 67.7(4) . . ?
C6 Os C1 36.8(4) . . ?
C4 Os C1 80.2(4) . . ?
C5 Os C1 67.8(4) . . ?
C15 N1 C11 117.6(9) . . ?
C15 N1 Os 118.2(7) . . ?
C11 N1 Os 123.2(8) . . ?
C17 N2 C16 116.7(9) . . ?
C17 N2 Os 127.8(8) . . ?
C16 N2 Os 115.1(7) . . ?
C17 N3 C18 130.0(10) . . ?
C17 N3 H3N 108(8) . . ?
C18 N3 H3N 122(8) . . ?
C17 N4 C25 124.6(10) . . ?
C17 N4 H4N 122(9) . . ?
C25 N4 H4N 113(9) . . ?
C32 N5 C36 118.7(10) . . ?
C32 N5 Os 123.7(7) . . ?
C36 N5 Os 117.5(7) . . ?
C6 C1 C2 117.8(11) . . ?
C6 C1 C7 122.1(11) . . ?
C2 C1 C7 120.0(11) . . ?
C6 C1 Os 70.3(6) . . ?
C2 C1 Os 69.6(6) . . ?
C7 C1 Os 130.8(8) . . ?
C3 C2 C1 120.5(11) . . ?
C3 C2 Os 71.6(6) . . ?
C1 C2 Os 72.3(6) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
Os C2 H2 128.7 . . ?
C2 C3 C4 121.8(10) . . ?
C2 C3 Os 71.4(6) . . ?
C4 C3 Os 72.6(6) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
Os C3 H3 129.5 . . ?
C5 C4 C3 119.2(10) . . ?
C5 C4 C8 121.7(10) . . ?
C3 C4 C8 119.1(9) . . ?
C5 C4 Os 71.7(6) . . ?
C3 C4 Os 70.3(6) . . ?
C8 C4 Os 128.7(7) . . ?
C4 C5 C6 119.4(10) . . ?
C4 C5 Os 71.5(6) . . ?
C6 C5 Os 69.7(6) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
Os C5 H5 131.2 . . ?
C1 C6 C5 121.3(10) . . ?
C1 C6 Os 72.9(7) . . ?
C5 C6 Os 72.0(6) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
Os C6 H6 128.0 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 C10 108.6(10) . . ?
C4 C8 C9 115.5(10) . . ?
C10 C8 C9 110.5(10) . . ?
C4 C8 H8 107.3 . . ?
C10 C8 H8 107.3 . . ?
C9 C8 H8 107.3 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 122.5(10) . . ?
N1 C11 H11 118.8 . . ?
C12 C11 H11 118.8 . . ?
C11 C12 C13 118.9(11) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C14 C13 C12 119.2(11) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C15 C14 C13 118.1(11) . . ?
C15 C14 H14 121.0 . . ?
C13 C14 H14 121.0 . . ?
N1 C15 C14 123.8(10) . . ?
N1 C15 C16 114.8(9) . . ?
C14 C15 C16 121.3(11) . . ?
N2 C16 C15 111.5(9) . . ?
N2 C16 H16A 109.3 . . ?
C15 C16 H16A 109.3 . . ?
N2 C16 H16B 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
N2 C17 N3 119.5(10) . . ?
N2 C17 N4 121.4(11) . . ?
N3 C17 N4 119.1(11) . . ?
C23 C18 C19 120.1(11) . . ?
C23 C18 N3 120.2(11) . . ?
C19 C18 N3 119.6(11) . . ?
C20 C19 C18 119.4(12) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 121.4(12) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C22 C21 C20 117.4(11) . . ?
C22 C21 C24 121.2(12) . . ?
C20 C21 C24 121.4(12) . . ?
C23 C22 C21 121.4(12) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C18 C23 C22 120.1(12) . . ?
C18 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C30 120.3(11) . . ?
C26 C25 N4 119.6(11) . . ?
C30 C25 N4 120.1(10) . . ?
C25 C26 C27 119.1(12) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.4 . . ?
C28 C27 C26 122.2(12) . . ?
C28 C27 H27 118.9 . . ?
C26 C27 H27 118.9 . . ?
C27 C28 C29 118.2(12) . . ?
C27 C28 C31 123.3(13) . . ?
C29 C28 C31 118.5(13) . . ?
C30 C29 C28 119.9(12) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C25 120.0(11) . . ?
C29 C30 H30 120.0 . . ?
C25 C30 H30 120.0 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N5 C32 C33 121.8(11) . . ?
N5 C32 H32 119.1 . . ?
C33 C32 H32 119.1 . . ?
C32 C33 C34 119.6(11) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C35 C34 C33 118.6(11) . . ?
C35 C34 H34 120.7 . . ?
C33 C34 H34 120.7 . . ?
C36 C35 C34 119.5(11) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
N5 C36 C35 121.8(10) . . ?
N5 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
F2 Sb1 F6 91.9(4) . . ?
F2 Sb1 F4 91.4(4) . . ?
F6 Sb1 F4 90.7(4) . . ?
F2 Sb1 F5 90.3(4) . . ?
F6 Sb1 F5 177.4(4) . . ?
F4 Sb1 F5 90.6(4) . . ?
F2 Sb1 F1 177.6(4) . . ?
F6 Sb1 F1 90.1(4) . . ?
F4 Sb1 F1 89.9(4) . . ?
F5 Sb1 F1 87.7(4) . . ?
F2 Sb1 F3 90.4(4) . . ?
F6 Sb1 F3 89.5(4) . . ?
F4 Sb1 F3 178.2(4) . . ?
F5 Sb1 F3 89.2(4) . . ?
F1 Sb1 F3 88.2(3) . . ?
F10 Sb2 F11 90.0(3) . . ?
F10 Sb2 F9 178.5(3) . . ?
F11 Sb2 F9 91.5(3) . . ?
F10 Sb2 F8 89.8(3) . . ?
F11 Sb2 F8 90.8(3) . . ?
F9 Sb2 F8 89.9(3) . . ?
F10 Sb2 F7 90.3(3) . . ?
F11 Sb2 F7 90.4(3) . . ?
F9 Sb2 F7 90.0(3) . . ?
F8 Sb2 F7 178.7(3) . . ?
F10 Sb2 F12 89.3(3) . . ?
F11 Sb2 F12 179.2(3) . . ?
F9 Sb2 F12 89.2(3) . . ?
F8 Sb2 F12 88.7(3) . . ?
F7 Sb2 F12 90.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 2.1(16) . . . . ?
C7 C1 C2 C3 -178.8(10) . . . . ?
Os C1 C2 C3 55.0(9) . . . . ?
C6 C1 C2 Os -52.9(9) . . . . ?
C7 C1 C2 Os 126.2(10) . . . . ?
C1 C2 C3 C4 -0.8(15) . . . . ?
Os C2 C3 C4 54.5(9) . . . . ?
C1 C2 C3 Os -55.3(9) . . . . ?
C2 C3 C4 C5 0.4(15) . . . . ?
Os C3 C4 C5 54.4(9) . . . . ?
C2 C3 C4 C8 -178.2(9) . . . . ?
Os C3 C4 C8 -124.2(9) . . . . ?
C2 C3 C4 Os -54.0(9) . . . . ?
C3 C4 C5 C6 -1.2(15) . . . . ?
C8 C4 C5 C6 177.3(10) . . . . ?
Os C4 C5 C6 52.5(9) . . . . ?
C3 C4 C5 Os -53.7(9) . . . . ?
C8 C4 C5 Os 124.8(10) . . . . ?
C2 C1 C6 C5 -2.9(16) . . . . ?
C7 C1 C6 C5 177.9(10) . . . . ?
Os C1 C6 C5 -55.5(9) . . . . ?
C2 C1 C6 Os 52.6(9) . . . . ?
C7 C1 C6 Os -126.5(11) . . . . ?
C4 C5 C6 C1 2.6(16) . . . . ?
Os C5 C6 C1 55.9(10) . . . . ?
C4 C5 C6 Os -53.3(9) . . . . ?
C5 C4 C8 C10 103.2(12) . . . . ?
C3 C4 C8 C10 -78.3(12) . . . . ?
Os C4 C8 C10 -165.6(8) . . . . ?
C5 C4 C8 C9 -21.6(15) . . . . ?
C3 C4 C8 C9 156.9(10) . . . . ?
Os C4 C8 C9 69.6(13) . . . . ?
C15 N1 C11 C12 1.2(16) . . . . ?
Os N1 C11 C12 -167.1(9) . . . . ?
N1 C11 C12 C13 0.2(18) . . . . ?
C11 C12 C13 C14 -1.9(18) . . . . ?
C12 C13 C14 C15 2.2(17) . . . . ?
C11 N1 C15 C14 -1.0(16) . . . . ?
Os N1 C15 C14 167.9(9) . . . . ?
C11 N1 C15 C16 176.7(10) . . . . ?
Os N1 C15 C16 -14.4(12) . . . . ?
C13 C14 C15 N1 -0.7(17) . . . . ?
C13 C14 C15 C16 -178.2(11) . . . . ?
C17 N2 C16 C15 171.7(9) . . . . ?
Os N2 C16 C15 -14.5(12) . . . . ?
N1 C15 C16 N2 18.6(14) . . . . ?
C14 C15 C16 N2 -163.7(10) . . . . ?
C16 N2 C17 N3 -169.3(10) . . . . ?
Os N2 C17 N3 17.8(15) . . . . ?
C16 N2 C17 N4 9.0(16) . . . . ?
Os N2 C17 N4 -163.9(8) . . . . ?
C18 N3 C17 N2 -148.9(11) . . . . ?
C18 N3 C17 N4 32.8(18) . . . . ?
C25 N4 C17 N2 -161.4(10) . . . . ?
C25 N4 C17 N3 16.9(17) . . . . ?
C17 N3 C18 C23 -146.5(13) . . . . ?
C17 N3 C18 C19 33.4(18) . . . . ?
C23 C18 C19 C20 4.5(17) . . . . ?
N3 C18 C19 C20 -175.5(10) . . . . ?
C18 C19 C20 C21 -2.1(18) . . . . ?
C19 C20 C21 C22 -1.9(18) . . . . ?
C19 C20 C21 C24 175.8(11) . . . . ?
C20 C21 C22 C23 3.6(19) . . . . ?
C24 C21 C22 C23 -174.1(12) . . . . ?
C19 C18 C23 C22 -2.8(19) . . . . ?
N3 C18 C23 C22 177.1(11) . . . . ?
C21 C22 C23 C18 -1(2) . . . . ?
C17 N4 C25 C26 -132.7(12) . . . . ?
C17 N4 C25 C30 46.6(16) . . . . ?
C30 C25 C26 C27 -3.9(17) . . . . ?
N4 C25 C26 C27 175.4(10) . . . . ?
C25 C26 C27 C28 -0.7(18) . . . . ?
C26 C27 C28 C29 3.4(18) . . . . ?
C26 C27 C28 C31 -178.4(12) . . . . ?
C27 C28 C29 C30 -1.4(19) . . . . ?
C31 C28 C29 C30 -179.8(12) . . . . ?
C28 C29 C30 C25 -3.1(19) . . . . ?
C26 C25 C30 C29 5.8(18) . . . . ?
N4 C25 C30 C29 -173.5(11) . . . . ?
C36 N5 C32 C33 0.7(17) . . . . ?
Os N5 C32 C33 -176.9(9) . . . . ?
N5 C32 C33 C34 0.4(19) . . . . ?
C32 C33 C34 C35 -1.5(19) . . . . ?
C33 C34 C35 C36 1.4(19) . . . . ?
C32 N5 C36 C35 -0.8(17) . . . . ?
Os N5 C36 C35 177.0(9) . . . . ?
C34 C35 C36 N5 -0.3(19) . . . . ?

_refine_diff_density_max         1.590
_refine_diff_density_min         -2.290
_refine_diff_density_rms         0.316

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cmpnd_11
_database_code_depnum_ccdc_archive 'CCDC 1983336'
loop_
_audit_author_name
_audit_author_address
'Pilar Garcia-Orduna'
;Instituto de Sintesis Quimica y Catalisis Homogenea (ISQCH, CSIC Univ Zaragoza)
Spain
;
_audit_update_record             
;
2020-07-31 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H43 N3 Os P, F6 Sb, C H2 Cl2'
_chemical_formula_sum            'C40 H45 Cl2 F6 N3 Os P Sb'
_chemical_formula_weight         1095.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   24.6016(11)
_cell_length_b                   10.2764(5)
_cell_length_c                   16.4397(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4156.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9627
_cell_measurement_theta_min      2.337
_cell_measurement_theta_max      28.523

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_F_000             2144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.325
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    3.931
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3161
_exptl_absorpt_correction_T_max  0.4546
_exptl_absorpt_process_details   
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.
;
_exptl_absorpt_special_details   ?


_diffrn_ambient_temperature      120(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 APEX CCD system'
_diffrn_measurement_method       'narrow ω frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_decay_%        0
_diffrn_reflns_number            53101
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.068
_diffrn_reflns_theta_max         28.655
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             9956
_reflns_number_gt                9428
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_max     0.899
_reflns_Friedel_fraction_full    0.987

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_cell_refinement       'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'


_refine_special_details          
;The asymmetric unit contains an osmium complex, a Sb F6 counterion and a 
solvent molecule (commented below). 

Most of the hydrogen atoms have been included in the model in calculated
positions and refined with a riding model. The one of the NH group has been 
included in observed position and refined with a geometrical restraint
concerning N-H bond length.

When convergence is achieved, the structure contains solvent accesible voids.
Residual density peaks are observed. Several tests (including disorder effects) 
have been performed to interpret them as a dichloromethane molecule. However, 
they lead to unrealistic atomic displacement parameters. An analysis of the
solvent region has been performed using SQUEEZE program. The contribution 
of the solvent have been calculated and incorporated in the further refinment.,SQUEEZE
;

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.443 0.052 -0.009 135 45 ' '
2 0.557 -0.052 0.491 135 45 ' '
3 0.943 0.448 -0.009 135 45 ' '
4 0.057 0.552 0.491 135 45 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
 The total potential solvent accesible void volume (540 Α3)  and the electron
 count (180  e in the unit cell) may agree with the presence of four 
 dichloromethane molecules  (C H2 Cl2). They have been included in the chemical 
 formula, F00 and density. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0190P)²+1.0039P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Direct method'
_atom_sites_solution_secondary   'Fourier Difference Synthesis'
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 4148 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9956
_refine_ls_number_parameters     469
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0232
_refine_ls_wR_factor_ref         0.0572
_refine_ls_wR_factor_gt          0.0557
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.28600(2) 0.93223(2) 0.49912(2) 0.01873(5) Uani 1 1 d . . . . .
P P 0.31108(5) 0.76998(11) 0.59075(7) 0.0204(2) Uani 1 1 d . . . . .
N1 N 0.30879(18) 1.0438(4) 0.6032(3) 0.0228(8) Uani 1 1 d . . . . .
N2 N 0.36494(15) 1.0116(3) 0.5026(3) 0.0236(7) Uani 1 1 d . . . . .
N3 N 0.40275(17) 1.1113(4) 0.6195(3) 0.0262(9) Uani 1 1 d D . . . .
C1 C 0.2352(2) 0.8078(4) 0.4172(3) 0.0246(10) Uani 1 1 d . . . . .
C2 C 0.2015(2) 0.8655(5) 0.4771(3) 0.0252(11) Uani 1 1 d . . . . .
H2 H 0.177471 0.812959 0.508282 0.030 Uiso 1 1 calc R U . . .
C3 C 0.20354(18) 1.0008(4) 0.4901(4) 0.0238(10) Uani 1 1 d . . . . .
H3 H 0.183425 1.036812 0.533960 0.029 Uiso 1 1 calc R U . . .
C4 C 0.2348(2) 1.0859(5) 0.4397(3) 0.0295(11) Uani 1 1 d . . . . .
C5 C 0.2676(2) 1.0270(5) 0.3797(3) 0.0259(10) Uani 1 1 d . . . . .
H5 H 0.288951 1.080301 0.344916 0.031 Uiso 1 1 calc R U . . .
C6 C 0.2695(2) 0.8874(5) 0.3702(3) 0.0268(10) Uani 1 1 d . . . . .
H6 H 0.293913 0.849397 0.332143 0.032 Uiso 1 1 calc R U . . .
C7 C 0.2339(3) 0.6637(5) 0.4020(4) 0.0361(13) Uani 1 1 d . . . . .
H7A H 0.231045 0.617532 0.454035 0.054 Uiso 1 1 calc R U . . .
H7B H 0.267371 0.637173 0.374221 0.054 Uiso 1 1 calc R U . . .
H7C H 0.202491 0.642271 0.367947 0.054 Uiso 1 1 calc R U . . .
C8 C 0.2348(2) 1.2311(5) 0.4571(4) 0.0325(11) Uani 1 1 d . . . . .
H8 H 0.242286 1.241802 0.516544 0.039 Uiso 1 1 calc R U . . .
C9 C 0.1789(2) 1.2896(6) 0.4410(4) 0.0413(14) Uani 1 1 d . . . . .
H9A H 0.171284 1.287311 0.382490 0.062 Uiso 1 1 calc R U . . .
H9B H 0.178220 1.379992 0.460027 0.062 Uiso 1 1 calc R U . . .
H9C H 0.151210 1.239237 0.470073 0.062 Uiso 1 1 calc R U . . .
C10 C 0.2797(3) 1.3044(6) 0.4113(6) 0.0535(19) Uani 1 1 d . . . . .
H10A H 0.314795 1.262647 0.421804 0.080 Uiso 1 1 calc R U . . .
H10B H 0.280884 1.394874 0.430121 0.080 Uiso 1 1 calc R U . . .
H10C H 0.272003 1.302553 0.352861 0.080 Uiso 1 1 calc R U . . .
C11 C 0.36978(19) 0.6690(4) 0.5684(3) 0.0228(10) Uani 1 1 d . . . . .
C12 C 0.3821(2) 0.6409(5) 0.4875(3) 0.0302(11) Uani 1 1 d . . . . .
H12 H 0.360692 0.676439 0.444815 0.036 Uiso 1 1 calc R U . . .
C13 C 0.4269(3) 0.5587(5) 0.4695(4) 0.0380(14) Uani 1 1 d . . . . .
H13 H 0.435027 0.537461 0.414590 0.046 Uiso 1 1 calc R U . . .
C14 C 0.4583(2) 0.5100(5) 0.5311(3) 0.0338(12) Uani 1 1 d . . . . .
H14 H 0.488896 0.457068 0.518679 0.041 Uiso 1 1 calc R U . . .
C15 C 0.4457(2) 0.5379(5) 0.6122(3) 0.0312(11) Uani 1 1 d . . . . .
H15 H 0.467389 0.503108 0.654719 0.037 Uiso 1 1 calc R U . . .
C16 C 0.4018(2) 0.6158(5) 0.6304(3) 0.0273(10) Uani 1 1 d . . . . .
H16 H 0.393194 0.633633 0.685579 0.033 Uiso 1 1 calc R U . . .
C17 C 0.25858(19) 0.6557(5) 0.6225(3) 0.0215(9) Uani 1 1 d . . . . .
C18 C 0.2644(2) 0.5207(5) 0.6152(3) 0.0239(10) Uani 1 1 d . . . . .
H18 H 0.296417 0.484649 0.592113 0.029 Uiso 1 1 calc R U . . .
C19 C 0.2225(2) 0.4392(5) 0.6422(4) 0.0296(12) Uani 1 1 d . . . . .
H19 H 0.226746 0.347488 0.638597 0.036 Uiso 1 1 calc R U . . .
C20 C 0.1755(2) 0.4897(5) 0.6739(3) 0.0298(11) Uani 1 1 d . . . . .
H20 H 0.146897 0.433393 0.690133 0.036 Uiso 1 1 calc R U . . .
C21 C 0.1699(2) 0.6229(6) 0.6822(3) 0.0309(11) Uani 1 1 d . . . . .
H21 H 0.137819 0.657871 0.705599 0.037 Uiso 1 1 calc R U . . .
C22 C 0.21087(19) 0.7055(5) 0.6565(3) 0.0270(11) Uani 1 1 d . . . . .
H22 H 0.206505 0.796908 0.662064 0.032 Uiso 1 1 calc R U . . .
C23 C 0.3285(2) 0.8542(5) 0.6865(3) 0.0278(11) Uani 1 1 d . . . . .
H23A H 0.315226 0.803483 0.733606 0.033 Uiso 1 1 calc R U . . .
H23B H 0.368478 0.863332 0.691256 0.033 Uiso 1 1 calc R U . . .
C24 C 0.3015(2) 0.9900(5) 0.6852(3) 0.0251(10) Uani 1 1 d . . . . .
H24A H 0.262294 0.982408 0.698084 0.030 Uiso 1 1 calc R U . . .
H24B H 0.318667 1.047518 0.726044 0.030 Uiso 1 1 calc R U . . .
C25 C 0.3601(2) 1.0612(4) 0.5769(3) 0.0234(10) Uani 1 1 d . . . . .
C26 C 0.4015(2) 1.0501(5) 0.4409(3) 0.0259(10) Uani 1 1 d . . . . .
C27 C 0.4116(2) 0.9666(5) 0.3774(3) 0.0273(10) Uani 1 1 d . . . . .
H27 H 0.396111 0.881962 0.377628 0.033 Uiso 1 1 calc R U . . .
C28 C 0.4444(2) 1.0049(6) 0.3126(3) 0.0337(12) Uani 1 1 d . . . . .
H28 H 0.450345 0.946039 0.268975 0.040 Uiso 1 1 calc R U . . .
C29 C 0.4686(2) 1.1271(6) 0.3102(4) 0.0382(13) Uani 1 1 d . . . . .
C30 C 0.4572(2) 1.2106(5) 0.3747(4) 0.0371(13) Uani 1 1 d . . . . .
H30 H 0.472433 1.295470 0.374212 0.044 Uiso 1 1 calc R U . . .
C31 C 0.4247(2) 1.1751(5) 0.4390(3) 0.0305(11) Uani 1 1 d . . . . .
H31 H 0.417886 1.234838 0.481942 0.037 Uiso 1 1 calc R U . . .
C32 C 0.5049(3) 1.1692(7) 0.2407(5) 0.058(2) Uani 1 1 d . . . . .
H32A H 0.496775 1.259626 0.226250 0.087 Uiso 1 1 calc R U . . .
H32B H 0.498482 1.113021 0.193517 0.087 Uiso 1 1 calc R U . . .
H32C H 0.543084 1.162233 0.257353 0.087 Uiso 1 1 calc R U . . .
C33 C 0.40202(19) 1.2030(4) 0.6840(3) 0.0242(10) Uani 1 1 d . . . . .
C34 C 0.4496(2) 1.2190(5) 0.7279(4) 0.0353(12) Uani 1 1 d . . . . .
H34 H 0.479969 1.165365 0.715720 0.042 Uiso 1 1 calc R U . . .
C35 C 0.4540(2) 1.3102(5) 0.7884(4) 0.0364(12) Uani 1 1 d . . . . .
H35 H 0.487151 1.319462 0.817406 0.044 Uiso 1 1 calc R U . . .
C36 C 0.4102(2) 1.3885(5) 0.8072(3) 0.0308(11) Uani 1 1 d . . . . .
C37 C 0.3620(2) 1.3723(5) 0.7645(3) 0.0273(10) Uani 1 1 d . . . . .
H37 H 0.331614 1.425304 0.777484 0.033 Uiso 1 1 calc R U . . .
C38 C 0.35744(19) 1.2801(4) 0.7029(3) 0.0243(10) Uani 1 1 d . . . . .
H38 H 0.324208 1.269954 0.674137 0.029 Uiso 1 1 calc R U . . .
C39 C 0.4161(3) 1.4940(6) 0.8723(4) 0.0433(15) Uani 1 1 d . . . . .
H39A H 0.417853 1.453358 0.926130 0.065 Uiso 1 1 calc R U . . .
H39B H 0.384758 1.552735 0.869877 0.065 Uiso 1 1 calc R U . . .
H39C H 0.449507 1.543577 0.862477 0.065 Uiso 1 1 calc R U . . .
Sb Sb 0.38837(2) 0.56782(3) 0.20900(2) 0.02582(8) Uani 1 1 d . . . . .
F1 F 0.44636(14) 0.4847(3) 0.2608(2) 0.0418(8) Uani 1 1 d . . . . .
F2 F 0.33013(15) 0.6518(3) 0.1575(2) 0.0501(10) Uani 1 1 d . . . . .
F3 F 0.39092(19) 0.7003(4) 0.2863(3) 0.0710(14) Uani 1 1 d . . . . .
F4 F 0.3846(2) 0.4346(3) 0.1318(3) 0.0586(12) Uani 1 1 d . . . . .
F5 F 0.33895(17) 0.4763(5) 0.2730(3) 0.0741(14) Uani 1 1 d . . . . .
F6 F 0.43695(18) 0.6553(4) 0.1426(3) 0.0736(14) Uani 1 1 d . . . . .
H3N H 0.4321(15) 1.099(5) 0.593(3) 0.018(13) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os N2 2.107(3) . ?
Os N1 2.134(4) . ?
Os C3 2.153(4) . ?
Os C6 2.207(5) . ?
Os C2 2.220(5) . ?
Os C5 2.237(5) . ?
Os C1 2.238(5) . ?
Os C4 2.244(5) . ?
Os P 2.3302(12) . ?
Os C25 2.592(5) . ?
P C11 1.816(5) . ?
P C17 1.822(5) . ?
P C23 1.846(5) . ?
N1 C25 1.347(7) . ?
N1 C24 1.468(6) . ?
N2 C25 1.329(7) . ?
N2 C26 1.413(7) . ?
N3 C25 1.363(7) . ?
N3 C33 1.418(6) . ?
N3 H3N 0.85(3) . ?
C1 C6 1.408(7) . ?
C1 C2 1.418(7) . ?
C1 C7 1.502(6) . ?
C2 C3 1.408(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.430(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.411(8) . ?
C4 C8 1.519(7) . ?
C5 C6 1.444(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.525(8) . ?
C8 C10 1.534(9) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.394(7) . ?
C11 C16 1.400(7) . ?
C12 C13 1.420(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.369(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.377(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.397(7) . ?
C17 C18 1.400(7) . ?
C18 C19 1.400(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.370(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.383(7) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.546(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 C27 1.375(7) . ?
C26 C31 1.405(6) . ?
C27 C28 1.391(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.390(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.393(8) . ?
C29 C32 1.514(8) . ?
C30 C31 1.375(7) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.384(7) . ?
C33 C38 1.388(6) . ?
C34 C35 1.372(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.380(8) . ?
C35 H35 0.9500 . ?
C36 C37 1.387(7) . ?
C36 C39 1.530(7) . ?
C37 C38 1.392(6) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
Sb F6 1.852(4) . ?
Sb F5 1.862(4) . ?
Sb F3 1.864(4) . ?
Sb F1 1.868(3) . ?
Sb F4 1.869(3) . ?
Sb F2 1.875(3) . ?

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 Os N1 61.85(17) . . ?
N2 Os C3 138.07(16) . . ?
N1 Os C3 97.31(19) . . ?
N2 Os C6 106.0(2) . . ?
N1 Os C6 158.47(17) . . ?
C3 Os C6 80.2(2) . . ?
N2 Os C2 170.96(18) . . ?
N1 Os C2 122.90(18) . . ?
C3 Os C2 37.52(19) . . ?
C6 Os C2 66.84(19) . . ?
N2 Os C5 92.38(19) . . ?
N1 Os C5 121.50(17) . . ?
C3 Os C5 66.8(2) . . ?
C6 Os C5 37.91(17) . . ?
C2 Os C5 78.58(18) . . ?
N2 Os C1 138.75(19) . . ?
N1 Os C1 159.36(18) . . ?
C3 Os C1 67.64(19) . . ?
C6 Os C1 36.92(19) . . ?
C2 Os C1 37.08(18) . . ?
C5 Os C1 66.95(18) . . ?
N2 Os C4 104.87(18) . . ?
N1 Os C4 96.81(18) . . ?
C3 Os C4 37.9(2) . . ?
C6 Os C4 68.01(19) . . ?
C2 Os C4 67.71(19) . . ?
C5 Os C4 36.7(2) . . ?
C1 Os C4 80.05(18) . . ?
N2 Os P 90.88(12) . . ?
N1 Os P 78.27(11) . . ?
C3 Os P 121.89(15) . . ?
C6 Os P 121.35(13) . . ?
C2 Os P 97.62(13) . . ?
C5 Os P 158.76(13) . . ?
C1 Os P 97.33(12) . . ?
C4 Os P 159.03(16) . . ?
N2 Os C25 30.71(18) . . ?
N1 Os C25 31.24(16) . . ?
C3 Os C25 121.99(17) . . ?
C6 Os C25 135.21(19) . . ?
C2 Os C25 153.88(17) . . ?
C5 Os C25 110.62(17) . . ?
C1 Os C25 169.04(18) . . ?
C4 Os C25 104.46(17) . . ?
P Os C25 82.00(11) . . ?
C11 P C17 104.7(2) . . ?
C11 P C23 104.8(2) . . ?
C17 P C23 102.9(2) . . ?
C11 P Os 119.23(16) . . ?
C17 P Os 117.29(16) . . ?
C23 P Os 106.08(17) . . ?
C25 N1 C24 117.4(4) . . ?
C25 N1 Os 93.5(3) . . ?
C24 N1 Os 120.1(3) . . ?
C25 N2 C26 127.5(4) . . ?
C25 N2 Os 95.2(3) . . ?
C26 N2 Os 132.6(4) . . ?
C25 N3 C33 128.7(4) . . ?
C25 N3 H3N 109(4) . . ?
C33 N3 H3N 120(4) . . ?
C6 C1 C2 119.3(4) . . ?
C6 C1 C7 119.7(5) . . ?
C2 C1 C7 121.0(5) . . ?
C6 C1 Os 70.4(3) . . ?
C2 C1 Os 70.8(3) . . ?
C7 C1 Os 132.5(4) . . ?
C3 C2 C1 119.8(4) . . ?
C3 C2 Os 68.6(2) . . ?
C1 C2 Os 72.1(3) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
Os C2 H2 132.0 . . ?
C2 C3 C4 122.4(5) . . ?
C2 C3 Os 73.8(3) . . ?
C4 C3 Os 74.5(3) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 H3 118.8 . . ?
Os C3 H3 124.5 . . ?
C5 C4 C3 116.8(5) . . ?
C5 C4 C8 123.6(5) . . ?
C3 C4 C8 119.4(5) . . ?
C5 C4 Os 71.4(3) . . ?
C3 C4 Os 67.6(3) . . ?
C8 C4 Os 127.5(4) . . ?
C4 C5 C6 121.4(5) . . ?
C4 C5 Os 71.9(3) . . ?
C6 C5 Os 69.9(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
Os C5 H5 131.9 . . ?
C1 C6 C5 119.9(5) . . ?
C1 C6 Os 72.7(3) . . ?
C5 C6 Os 72.2(3) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
Os C6 H6 127.0 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 C9 110.8(5) . . ?
C4 C8 C10 112.9(5) . . ?
C9 C8 C10 111.7(5) . . ?
C4 C8 H8 107.0 . . ?
C9 C8 H8 107.0 . . ?
C10 C8 H8 107.0 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 119.4(5) . . ?
C12 C11 P 119.0(4) . . ?
C16 C11 P 121.6(4) . . ?
C11 C12 C13 119.4(5) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C14 C13 C12 120.1(6) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.3(5) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 120.1(5) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C11 120.7(5) . . ?
C15 C16 H16 119.7 . . ?
C11 C16 H16 119.7 . . ?
C22 C17 C18 118.8(4) . . ?
C22 C17 P 118.3(4) . . ?
C18 C17 P 122.8(4) . . ?
C19 C18 C17 119.4(5) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C18 121.0(5) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C21 119.8(4) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 120.4(5) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C17 120.6(5) . . ?
C21 C22 H22 119.7 . . ?
C17 C22 H22 119.7 . . ?
C24 C23 P 108.1(3) . . ?
C24 C23 H23A 110.1 . . ?
P C23 H23A 110.1 . . ?
C24 C23 H23B 110.1 . . ?
P C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
N1 C24 C23 107.4(4) . . ?
N1 C24 H24A 110.2 . . ?
C23 C24 H24A 110.2 . . ?
N1 C24 H24B 110.2 . . ?
C23 C24 H24B 110.2 . . ?
H24A C24 H24B 108.5 . . ?
N2 C25 N1 109.1(4) . . ?
N2 C25 N3 123.3(5) . . ?
N1 C25 N3 127.4(5) . . ?
N2 C25 Os 54.1(2) . . ?
N1 C25 Os 55.3(2) . . ?
N3 C25 Os 171.4(3) . . ?
C27 C26 C31 118.7(5) . . ?
C27 C26 N2 119.0(4) . . ?
C31 C26 N2 122.1(4) . . ?
C26 C27 C28 120.6(5) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C29 C28 C27 121.7(5) . . ?
C29 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C28 C29 C30 116.6(5) . . ?
C28 C29 C32 122.2(6) . . ?
C30 C29 C32 121.2(6) . . ?
C31 C30 C29 122.7(5) . . ?
C31 C30 H30 118.7 . . ?
C29 C30 H30 118.7 . . ?
C30 C31 C26 119.7(5) . . ?
C30 C31 H31 120.2 . . ?
C26 C31 H31 120.2 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C38 118.9(5) . . ?
C34 C33 N3 117.2(4) . . ?
C38 C33 N3 123.8(4) . . ?
C35 C34 C33 121.7(5) . . ?
C35 C34 H34 119.1 . . ?
C33 C34 H34 119.1 . . ?
C34 C35 C36 120.0(5) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C37 118.9(5) . . ?
C35 C36 C39 119.7(5) . . ?
C37 C36 C39 121.4(5) . . ?
C36 C37 C38 121.3(5) . . ?
C36 C37 H37 119.3 . . ?
C38 C37 H37 119.3 . . ?
C33 C38 C37 119.2(4) . . ?
C33 C38 H38 120.4 . . ?
C37 C38 H38 120.4 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
F6 Sb F5 178.1(2) . . ?
F6 Sb F3 91.5(2) . . ?
F5 Sb F3 90.3(2) . . ?
F6 Sb F1 89.88(18) . . ?
F5 Sb F1 90.58(18) . . ?
F3 Sb F1 89.87(16) . . ?
F6 Sb F4 89.2(2) . . ?
F5 Sb F4 88.9(2) . . ?
F3 Sb F4 179.1(2) . . ?
F1 Sb F4 90.68(16) . . ?
F6 Sb F2 90.20(19) . . ?
F5 Sb F2 89.35(19) . . ?
F3 Sb F2 89.85(16) . . ?
F1 Sb F2 179.71(16) . . ?
F4 Sb F2 89.60(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -1.6(7) . . . . ?
C7 C1 C2 C3 180.0(5) . . . . ?
Os C1 C2 C3 51.3(4) . . . . ?
C6 C1 C2 Os -52.8(4) . . . . ?
C7 C1 C2 Os 128.7(5) . . . . ?
C1 C2 C3 C4 6.3(7) . . . . ?
Os C2 C3 C4 59.1(4) . . . . ?
C1 C2 C3 Os -52.9(4) . . . . ?
C2 C3 C4 C5 -5.3(7) . . . . ?
Os C3 C4 C5 53.5(4) . . . . ?
C2 C3 C4 C8 179.6(5) . . . . ?
Os C3 C4 C8 -121.6(5) . . . . ?
C2 C3 C4 Os -58.8(4) . . . . ?
C3 C4 C5 C6 -0.2(8) . . . . ?
C8 C4 C5 C6 174.7(5) . . . . ?
Os C4 C5 C6 51.5(4) . . . . ?
C3 C4 C5 Os -51.7(4) . . . . ?
C8 C4 C5 Os 123.2(5) . . . . ?
C2 C1 C6 C5 -3.7(7) . . . . ?
C7 C1 C6 C5 174.8(4) . . . . ?
Os C1 C6 C5 -56.7(4) . . . . ?
C2 C1 C6 Os 53.0(4) . . . . ?
C7 C1 C6 Os -128.5(4) . . . . ?
C4 C5 C6 C1 4.6(7) . . . . ?
Os C5 C6 C1 57.0(4) . . . . ?
C4 C5 C6 Os -52.4(5) . . . . ?
C5 C4 C8 C9 118.2(6) . . . . ?
C3 C4 C8 C9 -67.1(7) . . . . ?
Os C4 C8 C9 -150.2(4) . . . . ?
C5 C4 C8 C10 -8.0(8) . . . . ?
C3 C4 C8 C10 166.8(5) . . . . ?
Os C4 C8 C10 83.6(6) . . . . ?
C17 P C11 C12 101.6(4) . . . . ?
C23 P C11 C12 -150.4(4) . . . . ?
Os P C11 C12 -32.0(4) . . . . ?
C17 P C11 C16 -76.4(4) . . . . ?
C23 P C11 C16 31.5(4) . . . . ?
Os P C11 C16 150.0(3) . . . . ?
C16 C11 C12 C13 0.0(7) . . . . ?
P C11 C12 C13 -178.0(4) . . . . ?
C11 C12 C13 C14 -1.4(8) . . . . ?
C12 C13 C14 C15 1.8(9) . . . . ?
C13 C14 C15 C16 -0.7(8) . . . . ?
C14 C15 C16 C11 -0.7(8) . . . . ?
C12 C11 C16 C15 1.0(7) . . . . ?
P C11 C16 C15 179.0(4) . . . . ?
C11 P C17 C22 169.8(4) . . . . ?
C23 P C17 C22 60.4(4) . . . . ?
Os P C17 C22 -55.5(4) . . . . ?
C11 P C17 C18 -9.3(4) . . . . ?
C23 P C17 C18 -118.6(4) . . . . ?
Os P C17 C18 125.4(3) . . . . ?
C22 C17 C18 C19 -0.2(7) . . . . ?
P C17 C18 C19 178.9(4) . . . . ?
C17 C18 C19 C20 1.5(8) . . . . ?
C18 C19 C20 C21 -2.4(8) . . . . ?
C19 C20 C21 C22 1.9(8) . . . . ?
C20 C21 C22 C17 -0.5(8) . . . . ?
C18 C17 C22 C21 -0.4(7) . . . . ?
P C17 C22 C21 -179.5(4) . . . . ?
C11 P C23 C24 147.6(3) . . . . ?
C17 P C23 C24 -103.1(4) . . . . ?
Os P C23 C24 20.6(4) . . . . ?
C25 N1 C24 C23 -60.5(5) . . . . ?
Os N1 C24 C23 51.8(5) . . . . ?
P C23 C24 N1 -42.3(5) . . . . ?
C26 N2 C25 N1 152.7(4) . . . . ?
Os N2 C25 N1 -5.2(4) . . . . ?
C26 N2 C25 N3 -32.1(7) . . . . ?
Os N2 C25 N3 170.0(4) . . . . ?
C26 N2 C25 Os 157.9(5) . . . . ?
C24 N1 C25 N2 131.8(4) . . . . ?
Os N1 C25 N2 5.2(4) . . . . ?
C24 N1 C25 N3 -43.2(6) . . . . ?
Os N1 C25 N3 -169.8(4) . . . . ?
C24 N1 C25 Os 126.7(4) . . . . ?
C33 N3 C25 N2 156.9(5) . . . . ?
C33 N3 C25 N1 -28.8(8) . . . . ?
C25 N2 C26 C27 161.8(5) . . . . ?
Os N2 C26 C27 -48.8(7) . . . . ?
C25 N2 C26 C31 -23.4(8) . . . . ?
Os N2 C26 C31 126.1(5) . . . . ?
C31 C26 C27 C28 0.4(8) . . . . ?
N2 C26 C27 C28 175.4(5) . . . . ?
C26 C27 C28 C29 1.0(9) . . . . ?
C27 C28 C29 C30 -1.8(9) . . . . ?
C27 C28 C29 C32 179.2(6) . . . . ?
C28 C29 C30 C31 1.4(9) . . . . ?
C32 C29 C30 C31 -179.6(6) . . . . ?
C29 C30 C31 C26 -0.2(9) . . . . ?
C27 C26 C31 C30 -0.8(8) . . . . ?
N2 C26 C31 C30 -175.6(5) . . . . ?
C25 N3 C33 C34 167.5(5) . . . . ?
C25 N3 C33 C38 -15.2(8) . . . . ?
C38 C33 C34 C35 -1.1(8) . . . . ?
N3 C33 C34 C35 176.4(5) . . . . ?
C33 C34 C35 C36 0.3(9) . . . . ?
C34 C35 C36 C37 0.5(9) . . . . ?
C34 C35 C36 C39 -177.3(5) . . . . ?
C35 C36 C37 C38 -0.6(8) . . . . ?
C39 C36 C37 C38 177.2(5) . . . . ?
C34 C33 C38 C37 0.9(7) . . . . ?
N3 C33 C38 C37 -176.3(5) . . . . ?
C36 C37 C38 C33 -0.1(7) . . . . ?

_refine_diff_density_max         2.173
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.094





#===END
# ----------------------------------------------------------
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/hexane'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cmpnd_3
_database_code_depnum_ccdc_archive 'CCDC 1983332'
loop_
_audit_author_name
_audit_author_address
'Pilar Garcia-Orduna'
;Instituto de Sintesis Quimica y Catalisis Homogenea (ISQCH, CSIC Univ Zaragoza)
Spain
;
_audit_update_record             
;
2020-07-31 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C39 H45 Cl2 N3 P Os), 2(F6 Sb), 2(C H2 Cl2), 1.5(C6 H14)'
_chemical_formula_sum            'C89 H115 Cl8 F12 N6 Os2 P2 Sb2'
_chemical_formula_weight         2466.30

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0006(6)
_cell_length_b                   17.8189(9)
_cell_length_c                   26.0251(13)
_cell_angle_alpha                99.1650(10)
_cell_angle_beta                 100.6070(10)
_cell_angle_gamma                97.5640(10)
_cell_volume                     4881.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9835
_cell_measurement_theta_min      2.328
_cell_measurement_theta_max      28.343

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_F_000             2438
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    3.463
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5077
_exptl_absorpt_correction_T_max  0.6145
_exptl_absorpt_process_details   
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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 APEX CCD system'
_diffrn_measurement_method       'narrow ω frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            110689
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.910
_diffrn_reflns_theta_max         28.405
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             23468
_reflns_number_gt                19137
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_cell_refinement       'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'

_refine_special_details          
;
Asymmetric unit contains two molecules of an osmium complex, two SbF6 counterions,
two dichloromethane and one and a half hexane solvent molecules.
Most of the hydrogen atoms have been included in the model in 
calculated positions and refined with a riding model. Hydrogen
atoms of NH fragments have been observed in Fourier difference maps
and refined with restraints in N-H bond lengths.

At the end of the refinement, when convergence is achieved, highest
residual density peaks are observed close to the heaviest atoms
(Os and Sb). They have no chemical sense.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0516P)²+9.5797P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         23468
_refine_ls_number_parameters     1123
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0899
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.33424(2) 0.42731(2) 0.06096(2) 0.02389(5) Uani 1 1 d . . . . .
Cl1 Cl 0.27623(11) 0.55387(7) 0.05899(4) 0.0347(2) Uani 1 1 d . . . . .
Cl2 Cl 0.53253(9) 0.49713(6) 0.11556(4) 0.0303(2) Uani 1 1 d . . . . .
P1 P 0.26413(9) 0.42510(6) 0.14123(4) 0.0227(2) Uani 1 1 d . . . . .
N1 N 0.3433(5) 0.6437(2) 0.23118(16) 0.0414(10) Uani 1 1 d D . . . .
N2 N 0.4583(5) 0.6879(3) 0.17272(17) 0.0552(14) Uani 1 1 d D . . . .
N3 N 0.4881(4) 0.7563(2) 0.25894(16) 0.0411(10) Uani 1 1 d D . . . .
C1 C 0.1954(4) 0.3758(3) -0.01309(17) 0.0340(10) Uani 1 1 d . . . . .
C2 C 0.3066(4) 0.4099(3) -0.02704(17) 0.0331(10) Uani 1 1 d . . . . .
H2 H 0.3011 0.4462 -0.0500 0.040 Uiso 1 1 calc R U . . .
C3 C 0.4235(4) 0.3908(3) -0.00760(17) 0.0302(9) Uani 1 1 d . . . . .
H3 H 0.4959 0.4138 -0.0180 0.036 Uiso 1 1 calc R U . . .
C4 C 0.4353(4) 0.3371(3) 0.02789(17) 0.0295(9) Uani 1 1 d . . . . .
C5 C 0.3259(4) 0.3022(3) 0.04145(17) 0.0296(9) Uani 1 1 d . . . . .
H5 H 0.3313 0.2654 0.0642 0.036 Uiso 1 1 calc R U . . .
C6 C 0.2078(4) 0.3218(3) 0.02124(17) 0.0334(10) Uani 1 1 d . . . . .
H6 H 0.1351 0.2980 0.0310 0.040 Uiso 1 1 calc R U . . .
C7 C 0.0707(5) 0.3977(4) -0.0355(2) 0.0462(13) Uani 1 1 d . . . . .
H7A H 0.0043 0.3702 -0.0217 0.069 Uiso 1 1 calc R U . . .
H7B H 0.0526 0.3836 -0.0744 0.069 Uiso 1 1 calc R U . . .
H7C H 0.0745 0.4534 -0.0249 0.069 Uiso 1 1 calc R U . . .
C8 C 0.5641(4) 0.3182(3) 0.04774(19) 0.0335(10) Uani 1 1 d . . . . .
H8 H 0.6254 0.3673 0.0559 0.040 Uiso 1 1 calc R U . . .
C9 C 0.5770(5) 0.2837(3) 0.0980(2) 0.0449(12) Uani 1 1 d . . . . .
H9A H 0.5533 0.3185 0.1262 0.067 Uiso 1 1 calc R U . . .
H9B H 0.6641 0.2767 0.1094 0.067 Uiso 1 1 calc R U . . .
H9C H 0.5218 0.2337 0.0906 0.067 Uiso 1 1 calc R U . . .
C10 C 0.5984(6) 0.2646(4) 0.0022(2) 0.0505(14) Uani 1 1 d . . . . .
H10A H 0.5415 0.2151 -0.0060 0.076 Uiso 1 1 calc R U . . .
H10B H 0.6849 0.2560 0.0129 0.076 Uiso 1 1 calc R U . . .
H10C H 0.5908 0.2884 -0.0295 0.076 Uiso 1 1 calc R U . . .
C11 C 0.3326(4) 0.5056(3) 0.19685(17) 0.0291(9) Uani 1 1 d . . . . .
H11A H 0.3242 0.4889 0.2307 0.035 Uiso 1 1 calc R U . . .
H11B H 0.4232 0.5195 0.1977 0.035 Uiso 1 1 calc R U . . .
C12 C 0.2705(5) 0.5766(3) 0.19274(18) 0.0351(10) Uani 1 1 d . . . . .
H12A H 0.2634 0.5875 0.1563 0.042 Uiso 1 1 calc R U . . .
H12B H 0.1848 0.5665 0.1996 0.042 Uiso 1 1 calc R U . . .
C13 C 0.2969(4) 0.3403(3) 0.16909(17) 0.0295(9) Uani 1 1 d . . . . .
C14 C 0.2110(5) 0.2726(3) 0.15492(19) 0.0340(10) Uani 1 1 d . . . . .
H14 H 0.1330 0.2707 0.1315 0.041 Uiso 1 1 calc R U . . .
C15 C 0.2379(5) 0.2068(3) 0.1748(2) 0.0470(13) Uani 1 1 d . . . . .
H15 H 0.1786 0.1605 0.1648 0.056 Uiso 1 1 calc R U . . .
C16 C 0.3508(6) 0.2095(4) 0.2089(2) 0.0541(15) Uani 1 1 d . . . . .
H16 H 0.3694 0.1651 0.2228 0.065 Uiso 1 1 calc R U . . .
C17 C 0.4372(6) 0.2773(4) 0.2229(2) 0.0542(16) Uani 1 1 d . . . . .
H17 H 0.5155 0.2791 0.2461 0.065 Uiso 1 1 calc R U . . .
C18 C 0.4097(5) 0.3423(3) 0.2034(2) 0.0407(12) Uani 1 1 d . . . . .
H18 H 0.4689 0.3887 0.2136 0.049 Uiso 1 1 calc R U . . .
C19 C 0.0969(4) 0.4222(2) 0.13956(17) 0.0237(8) Uani 1 1 d . . . . .
C20 C 0.0523(4) 0.4117(3) 0.18510(18) 0.0287(9) Uani 1 1 d . . . . .
H20 H 0.1067 0.4017 0.2152 0.034 Uiso 1 1 calc R U . . .
C21 C -0.0723(4) 0.4161(3) 0.18624(19) 0.0323(10) Uani 1 1 d . . . . .
H21 H -0.1022 0.4106 0.2177 0.039 Uiso 1 1 calc R U . . .
C22 C -0.1528(4) 0.4283(3) 0.1425(2) 0.0382(11) Uani 1 1 d . . . . .
H22 H -0.2382 0.4302 0.1436 0.046 Uiso 1 1 calc R U . . .
C23 C -0.1100(4) 0.4378(3) 0.0969(2) 0.0439(13) Uani 1 1 d . . . . .
H23 H -0.1658 0.4456 0.0665 0.053 Uiso 1 1 calc R U . . .
C24 C 0.0164(4) 0.4356(3) 0.09588(19) 0.0327(10) Uani 1 1 d . . . . .
H24 H 0.0468 0.4435 0.0650 0.039 Uiso 1 1 calc R U . . .
C25 C 0.4299(6) 0.6957(3) 0.22111(19) 0.0432(13) Uani 1 1 d . . . . .
C26 C 0.5399(6) 0.7442(3) 0.15483(19) 0.0484(14) Uani 1 1 d . . . . .
C27 C 0.6261(6) 0.7190(3) 0.12759(19) 0.0506(15) Uani 1 1 d . . . . .
H27 H 0.6339 0.6660 0.1219 0.061 Uiso 1 1 calc R U . . .
C28 C 0.7025(6) 0.7716(3) 0.10827(19) 0.0508(15) Uani 1 1 d . . . . .
H28 H 0.7616 0.7538 0.0888 0.061 Uiso 1 1 calc R U . . .
C29 C 0.6941(6) 0.8492(3) 0.1169(2) 0.0494(14) Uani 1 1 d . . . . .
C30 C 0.6058(6) 0.8726(3) 0.1444(2) 0.0506(14) Uani 1 1 d . . . . .
H30 H 0.5987 0.9256 0.1507 0.061 Uiso 1 1 calc R U . . .
C31 C 0.5272(6) 0.8210(3) 0.1630(2) 0.0508(14) Uani 1 1 d . . . . .
H31 H 0.4655 0.8381 0.1811 0.061 Uiso 1 1 calc R U . . .
C32 C 0.7805(6) 0.9057(4) 0.0972(3) 0.0655(19) Uani 1 1 d . . . . .
H32A H 0.7391 0.9136 0.0622 0.098 Uiso 1 1 calc R U . . .
H32B H 0.8579 0.8853 0.0942 0.098 Uiso 1 1 calc R U . . .
H32C H 0.8005 0.9550 0.1223 0.098 Uiso 1 1 calc R U . . .
C33 C 0.4547(4) 0.7714(2) 0.30991(18) 0.0314(10) Uani 1 1 d . . . . .
C34 C 0.5398(4) 0.7691(2) 0.35544(18) 0.0294(9) Uani 1 1 d . . . . .
H34 H 0.6221 0.7599 0.3534 0.035 Uiso 1 1 calc R U . . .
C35 C 0.5044(4) 0.7804(2) 0.40445(18) 0.0286(9) Uani 1 1 d . . . . .
H35 H 0.5637 0.7799 0.4359 0.034 Uiso 1 1 calc R U . . .
C36 C 0.3841(4) 0.7923(2) 0.40811(18) 0.0285(9) Uani 1 1 d . . . . .
C37 C 0.3009(4) 0.7968(2) 0.3619(2) 0.0351(11) Uani 1 1 d . . . . .
H37 H 0.2191 0.8066 0.3641 0.042 Uiso 1 1 calc R U . . .
C38 C 0.3338(4) 0.7874(3) 0.31301(18) 0.0333(10) Uani 1 1 d . . . . .
H38 H 0.2762 0.7916 0.2820 0.040 Uiso 1 1 calc R U . . .
C39 C 0.3439(5) 0.7972(3) 0.4605(2) 0.0368(11) Uani 1 1 d . . . . .
H39A H 0.4105 0.7855 0.4871 0.055 Uiso 1 1 calc R U . . .
H39B H 0.2672 0.7600 0.4564 0.055 Uiso 1 1 calc R U . . .
H39C H 0.3278 0.8494 0.4721 0.055 Uiso 1 1 calc R U . . .
Os51 Os 0.08129(2) 0.29819(2) 0.47498(2) 0.02146(5) Uani 1 1 d . . . . .
Cl51 Cl -0.11388(10) 0.20951(6) 0.45916(5) 0.0312(2) Uani 1 1 d . . . . .
Cl52 Cl 0.17921(10) 0.20054(6) 0.51458(4) 0.0273(2) Uani 1 1 d . . . . .
P51 P 0.11213(9) 0.23161(6) 0.39363(4) 0.0209(2) Uani 1 1 d . . . . .
N51 N -0.0766(3) 0.00673(19) 0.35320(14) 0.0247(7) Uani 1 1 d D . . . .
H51N H -0.0498 -0.0263 0.3311 0.030 Uiso 1 1 d DR U . . .
N52 N -0.1429(3) 0.02828(19) 0.43237(14) 0.0244(7) Uani 1 1 d D . . . .
N53 N -0.1536(3) -0.09749(19) 0.38818(14) 0.0234(7) Uani 1 1 d D . . . .
C51 C -0.0238(4) 0.3959(2) 0.4759(2) 0.0328(10) Uani 1 1 d . . . . .
C52 C 0.0075(4) 0.3829(2) 0.5292(2) 0.0330(10) Uani 1 1 d . . . . .
H52 H -0.0567 0.3761 0.5488 0.040 Uiso 1 1 calc R U . . .
C53 C 0.1305(4) 0.3800(2) 0.55293(18) 0.0299(9) Uani 1 1 d . . . . .
H53 H 0.1488 0.3713 0.5884 0.036 Uiso 1 1 calc R U . . .
C54 C 0.2311(4) 0.3901(2) 0.52449(17) 0.0248(8) Uani 1 1 d . . . . .
C55 C 0.2011(4) 0.4054(2) 0.47269(17) 0.0246(8) Uani 1 1 d . . . . .
H55 H 0.2659 0.4140 0.4537 0.030 Uiso 1 1 calc R U . . .
C56 C 0.0744(4) 0.4082(2) 0.44804(19) 0.0296(9) Uani 1 1 d . . . . .
H56 H 0.0561 0.4184 0.4129 0.036 Uiso 1 1 calc R U . . .
C57 C -0.1585(4) 0.3985(3) 0.4512(2) 0.0432(13) Uani 1 1 d . . . . .
H57A H -0.1868 0.4419 0.4712 0.065 Uiso 1 1 calc R U . . .
H57B H -0.2115 0.3502 0.4522 0.065 Uiso 1 1 calc R U . . .
H57C H -0.1645 0.4049 0.4142 0.065 Uiso 1 1 calc R U . . .
C58 C 0.3641(4) 0.3906(2) 0.55307(17) 0.0286(9) Uani 1 1 d . . . . .
H58 H 0.3609 0.3532 0.5778 0.034 Uiso 1 1 calc R U . . .
C59 C 0.4138(5) 0.4711(3) 0.5870(2) 0.0375(11) Uani 1 1 d . . . . .
H59A H 0.4205 0.5089 0.5637 0.056 Uiso 1 1 calc R U . . .
H59B H 0.4967 0.4715 0.6088 0.056 Uiso 1 1 calc R U . . .
H59C H 0.3561 0.4844 0.6102 0.056 Uiso 1 1 calc R U . . .
C60 C 0.4512(4) 0.3670(3) 0.51649(19) 0.0350(10) Uani 1 1 d . . . . .
H60A H 0.4138 0.3172 0.4935 0.052 Uiso 1 1 calc R U . . .
H60B H 0.5322 0.3627 0.5380 0.052 Uiso 1 1 calc R U . . .
H60C H 0.4637 0.4060 0.4945 0.052 Uiso 1 1 calc R U . . .
C61 C 0.0819(4) 0.1250(2) 0.38310(16) 0.0230(8) Uani 1 1 d . . . . .
H61A H 0.1443 0.1047 0.3641 0.028 Uiso 1 1 calc R U . . .
H61B H 0.0944 0.1092 0.4182 0.028 Uiso 1 1 calc R U . . .
C62 C -0.0500(4) 0.0884(2) 0.35140(17) 0.0247(8) Uani 1 1 d . . . . .
H62A H -0.1127 0.1153 0.3663 0.030 Uiso 1 1 calc R U . . .
H62B H -0.0573 0.0948 0.3139 0.030 Uiso 1 1 calc R U . . .
C63 C 0.2718(4) 0.2536(2) 0.38416(16) 0.0225(8) Uani 1 1 d . . . . .
C64 C 0.3069(4) 0.3172(3) 0.36168(18) 0.0307(9) Uani 1 1 d . . . . .
H64 H 0.2463 0.3477 0.3501 0.037 Uiso 1 1 calc R U . . .
C65 C 0.4298(4) 0.3360(3) 0.35622(19) 0.0358(11) Uani 1 1 d . . . . .
H65 H 0.4534 0.3792 0.3409 0.043 Uiso 1 1 calc R U . . .
C66 C 0.5183(4) 0.2915(3) 0.3732(2) 0.0392(11) Uani 1 1 d . . . . .
H66 H 0.6022 0.3043 0.3692 0.047 Uiso 1 1 calc R U . . .
C67 C 0.4854(4) 0.2289(3) 0.39593(18) 0.0345(10) Uani 1 1 d . . . . .
H67 H 0.5463 0.1987 0.4075 0.041 Uiso 1 1 calc R U . . .
C68 C 0.3620(4) 0.2103(2) 0.40172(17) 0.0278(9) Uani 1 1 d . . . . .
H68 H 0.3394 0.1677 0.4178 0.033 Uiso 1 1 calc R U . . .
C69 C 0.0155(4) 0.2485(2) 0.33289(17) 0.0266(9) Uani 1 1 d . . . . .
C70 C 0.0464(4) 0.2280(3) 0.28342(18) 0.0340(10) Uani 1 1 d . . . . .
H70 H 0.1249 0.2123 0.2814 0.041 Uiso 1 1 calc R U . . .
C71 C -0.0377(5) 0.2306(3) 0.2374(2) 0.0459(13) Uani 1 1 d . . . . .
H71 H -0.0168 0.2166 0.2037 0.055 Uiso 1 1 calc R U . . .
C72 C -0.1527(5) 0.2537(3) 0.2400(2) 0.0464(13) Uani 1 1 d . . . . .
H72 H -0.2104 0.2551 0.2083 0.056 Uiso 1 1 calc R U . . .
C73 C -0.1823(5) 0.2744(3) 0.2887(2) 0.0426(12) Uani 1 1 d . . . . .
H73 H -0.2603 0.2909 0.2904 0.051 Uiso 1 1 calc R U . . .
C74 C -0.1003(4) 0.2716(3) 0.3353(2) 0.0329(10) Uani 1 1 d . . . . .
H74 H -0.1225 0.2854 0.3687 0.039 Uiso 1 1 calc R U . . .
C75 C -0.1243(4) -0.0207(2) 0.39101(16) 0.0220(8) Uani 1 1 d . . . . .
C76 C -0.2013(4) 0.0102(2) 0.47436(16) 0.0238(8) Uani 1 1 d . . . . .
C77 C -0.1403(4) 0.0463(2) 0.52607(17) 0.0257(8) Uani 1 1 d . . . . .
H77 H -0.0596 0.0768 0.5321 0.031 Uiso 1 1 calc R U . . .
C78 C -0.1966(4) 0.0379(2) 0.56829(17) 0.0280(9) Uani 1 1 d . . . . .
H78 H -0.1546 0.0627 0.6033 0.034 Uiso 1 1 calc R U . . .
C79 C -0.3156(4) -0.0070(2) 0.56001(17) 0.0276(9) Uani 1 1 d . . . . .
C80 C -0.3721(4) -0.0437(2) 0.50850(18) 0.0268(9) Uani 1 1 d . . . . .
H80 H -0.4514 -0.0758 0.5024 0.032 Uiso 1 1 calc R U . . .
C81 C -0.3171(4) -0.0350(2) 0.46550(17) 0.0244(8) Uani 1 1 d . . . . .
H81 H -0.3589 -0.0599 0.4305 0.029 Uiso 1 1 calc R U . . .
C82 C -0.3794(5) -0.0113(3) 0.60628(19) 0.0347(10) Uani 1 1 d . . . . .
H82A H -0.4626 -0.0432 0.5936 0.052 Uiso 1 1 calc R U . . .
H82B H -0.3882 0.0407 0.6225 0.052 Uiso 1 1 calc R U . . .
H82C H -0.3289 -0.0343 0.6328 0.052 Uiso 1 1 calc R U . . .
C83 C -0.1370(4) -0.1535(2) 0.34489(16) 0.0228(8) Uani 1 1 d . . . . .
C84 C -0.0669(4) -0.2106(2) 0.35567(17) 0.0253(8) Uani 1 1 d . . . . .
H84 H -0.0331 -0.2143 0.3913 0.030 Uiso 1 1 calc R U . . .
C85 C -0.0470(4) -0.2626(3) 0.31313(18) 0.0312(9) Uani 1 1 d . . . . .
H85 H 0.0003 -0.3021 0.3203 0.037 Uiso 1 1 calc R U . . .
C86 C -0.0949(4) -0.2582(3) 0.26028(19) 0.0332(10) Uani 1 1 d . . . . .
C87 C -0.1663(4) -0.2017(3) 0.25105(17) 0.0299(9) Uani 1 1 d . . . . .
H87 H -0.2003 -0.1980 0.2154 0.036 Uiso 1 1 calc R U . . .
C88 C -0.1896(4) -0.1501(2) 0.29266(17) 0.0267(9) Uani 1 1 d . . . . .
H88 H -0.2412 -0.1126 0.2855 0.032 Uiso 1 1 calc R U . . .
C89 C -0.0676(6) -0.3119(3) 0.2148(2) 0.0480(13) Uani 1 1 d . . . . .
H89A H -0.1466 -0.3391 0.1914 0.072 Uiso 1 1 calc R U . . .
H89B H -0.0194 -0.3495 0.2287 0.072 Uiso 1 1 calc R U . . .
H89C H -0.0188 -0.2823 0.1946 0.072 Uiso 1 1 calc R U . . .
Sb1 Sb 0.11701(3) 0.96821(2) 0.22858(2) 0.03496(8) Uani 1 1 d . . . . .
F1 F 0.2109(3) 1.06122(18) 0.27030(13) 0.0537(8) Uani 1 1 d . . . . .
F2 F 0.0254(3) 0.87576(18) 0.18753(12) 0.0493(8) Uani 1 1 d . . . . .
F3 F 0.1281(4) 1.0075(2) 0.16741(13) 0.0686(11) Uani 1 1 d . . . . .
F4 F 0.1038(3) 0.9327(2) 0.29175(12) 0.0624(10) Uani 1 1 d . . . . .
F5 F 0.2657(3) 0.9280(2) 0.22758(14) 0.0558(9) Uani 1 1 d . . . . .
F6 F -0.0319(3) 1.0065(3) 0.23238(16) 0.0789(13) Uani 1 1 d . . . . .
Sb2 Sb 0.17619(3) 0.55078(2) 0.34422(2) 0.03112(7) Uani 1 1 d . . . . .
F7 F 0.3292(3) 0.59974(17) 0.33400(12) 0.0458(7) Uani 1 1 d . . . . .
F8 F 0.0202(3) 0.50274(19) 0.35187(13) 0.0544(8) Uani 1 1 d . . . . .
F9 F 0.2068(3) 0.45807(17) 0.30803(12) 0.0542(9) Uani 1 1 d . . . . .
F10 F 0.1472(3) 0.64422(17) 0.38022(12) 0.0450(7) Uani 1 1 d . . . . .
F11 F 0.2548(3) 0.52845(17) 0.40858(11) 0.0399(7) Uani 1 1 d . . . . .
F12 F 0.0972(3) 0.57422(18) 0.27993(11) 0.0498(8) Uani 1 1 d . . . . .
C41 C 0.7452(7) 0.5426(4) 0.2659(3) 0.0643(18) Uani 1 1 d . . . . .
H41A H 0.8345 0.5646 0.2808 0.077 Uiso 1 1 calc R U . . .
H41B H 0.7309 0.5373 0.2267 0.077 Uiso 1 1 calc R U . . .
Cl3 Cl 0.71262(13) 0.45070(8) 0.28234(6) 0.0526(3) Uani 1 1 d . . . . .
Cl4 Cl 0.65141(15) 0.60542(9) 0.29048(7) 0.0576(4) Uani 1 1 d . . . . .
C42 C 0.4869(6) -0.0410(4) 0.7261(3) 0.0661(18) Uani 1 1 d . . . . .
H42A H 0.5582 -0.0179 0.7561 0.079 Uiso 0.524(11) 1 calc R U P A 3
H42B H 0.5181 -0.0762 0.6999 0.079 Uiso 0.524(11) 1 calc R U P A 3
H42C H 0.5501 -0.0609 0.7074 0.079 Uiso 0.476(11) 1 calc R U P A 4
H42D H 0.5293 -0.0191 0.7635 0.079 Uiso 0.476(11) 1 calc R U P A 4
Cl5A Cl 0.3688(4) -0.0942(4) 0.7500(3) 0.0898(18) Uiso 0.524(11) 1 d . . P A 3
Cl5B Cl 0.3701(3) -0.1163(2) 0.7251(2) 0.0573(15) Uiso 0.476(11) 1 d . . P A 4
Cl6 Cl 0.42933(16) 0.03249(10) 0.69586(7) 0.0637(4) Uani 1 1 d . . . . .
C45 C 0.1818(7) 0.7543(4) 0.1269(3) 0.077(2) Uani 1 1 d . . . . .
H45A H 0.0972 0.7506 0.1343 0.116 Uiso 1 1 calc R U . . .
H45B H 0.2438 0.7661 0.1606 0.116 Uiso 1 1 calc R U . . .
H45C H 0.1909 0.7051 0.1062 0.116 Uiso 1 1 calc R U . . .
C46 C 0.2028(7) 0.8184(5) 0.0951(3) 0.076(2) Uani 1 1 d . . . . .
H46A H 0.1998 0.8684 0.1174 0.091 Uiso 1 1 calc R U . . .
H46B H 0.2876 0.8208 0.0871 0.091 Uiso 1 1 calc R U . . .
C47 C 0.1086(7) 0.8076(4) 0.0442(3) 0.075(2) Uani 1 1 d . . . . .
H47A H 0.1108 0.7572 0.0224 0.090 Uiso 1 1 calc R U . . .
H47B H 0.0241 0.8058 0.0525 0.090 Uiso 1 1 calc R U . . .
C48 C 0.1271(9) 0.8683(6) 0.0119(4) 0.107(3) Uani 1 1 d . . . . .
H48A H 0.1973 0.8585 -0.0058 0.128 Uiso 0.593(18) 1 calc R U P B 1
H48B H 0.1547 0.9183 0.0369 0.128 Uiso 0.593(18) 1 calc R U P B 1
H48C H 0.2181 0.8831 0.0140 0.128 Uiso 0.407(18) 1 calc R U P B 2
H48D H 0.0961 0.9145 0.0278 0.128 Uiso 0.407(18) 1 calc R U P B 2
C49A C 0.013(2) 0.8782(14) -0.0325(8) 0.133(8) Uiso 0.593(18) 1 d D . P B 1
H49A H -0.0262 0.9229 -0.0205 0.160 Uiso 0.593(18) 1 calc R U P B 1
H49B H -0.0513 0.8311 -0.0433 0.160 Uiso 0.593(18) 1 calc R U P B 1
C50A C 0.0861(16) 0.8930(11) -0.0811(7) 0.105(6) Uiso 0.593(18) 1 d D . P B 1
H50A H 0.1545 0.9369 -0.0680 0.158 Uiso 0.593(18) 1 calc R U P B 1
H50B H 0.0266 0.9040 -0.1108 0.158 Uiso 0.593(18) 1 calc R U P B 1
H50C H 0.1204 0.8469 -0.0932 0.158 Uiso 0.593(18) 1 calc R U P B 1
C49B C 0.0573(16) 0.8432(10) -0.0502(6) 0.056(5) Uiso 0.407(18) 1 d . . P B 2
H49C H -0.0245 0.8092 -0.0555 0.068 Uiso 0.407(18) 1 calc R U P B 2
H49D H 0.1104 0.8189 -0.0726 0.068 Uiso 0.407(18) 1 calc R U P B 2
C50B C 0.041(2) 0.9369(15) -0.0603(10) 0.099(9) Uiso 0.407(18) 1 d . . P B 2
H50D H 0.0551 0.9716 -0.0258 0.149 Uiso 0.407(18) 1 calc R U P B 2
H50E H -0.0438 0.9365 -0.0803 0.149 Uiso 0.407(18) 1 calc R U P B 2
H50F H 0.1025 0.9548 -0.0804 0.149 Uiso 0.407(18) 1 calc R U P B 2
C95 C 0.4944(10) 1.0061(7) 0.0283(4) 0.116(4) Uani 1 1 d . . . . .
H95A H 0.4871 0.9545 0.0381 0.140 Uiso 1 1 calc R U . . .
H95B H 0.5762 1.0353 0.0490 0.140 Uiso 1 1 calc R U . . .
C96 C 0.4007(12) 1.0429(8) 0.0490(5) 0.138(5) Uani 1 1 d . . . . .
H96A H 0.3177 1.0172 0.0272 0.165 Uiso 1 1 calc R U . . .
H96B H 0.4124 1.0969 0.0436 0.165 Uiso 1 1 calc R U . . .
C97 C 0.3962(12) 1.0441(6) 0.1050(4) 0.132(4) Uani 1 1 d . . . . .
H97A H 0.3683 0.9917 0.1099 0.198 Uiso 1 1 calc R U . . .
H97B H 0.3374 1.0775 0.1153 0.198 Uiso 1 1 calc R U . . .
H97C H 0.4800 1.0638 0.1272 0.198 Uiso 1 1 calc R U . . .
H52N H -0.108(4) 0.0755(14) 0.4348(18) 0.024(12) Uiso 1 1 d D . . . .
H53N H -0.165(4) -0.109(2) 0.4178(11) 0.021(11) Uiso 1 1 d D . . . .
H1N H 0.354(5) 0.641(3) 0.2646(9) 0.046(16) Uiso 1 1 d D . . . .
H2N H 0.437(6) 0.6432(19) 0.152(2) 0.061(19) Uiso 1 1 d D . . . .
H3N H 0.555(4) 0.783(3) 0.252(2) 0.057(18) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C6 2.169(5) . ?
Os1 C5 2.193(4) . ?
Os1 C1 2.207(4) . ?
Os1 C2 2.219(4) . ?
Os1 C4 2.224(4) . ?
Os1 C3 2.239(4) . ?
Os1 P1 2.3605(10) . ?
Os1 Cl1 2.4288(11) . ?
Os1 Cl2 2.4304(10) . ?
P1 C19 1.826(4) . ?
P1 C13 1.827(5) . ?
P1 C11 1.837(4) . ?
N1 C25 1.330(6) . ?
N1 C12 1.465(6) . ?
N1 H1N 0.865(19) . ?
N2 C25 1.343(7) . ?
N2 C26 1.447(6) . ?
N2 H2N 0.86(2) . ?
N3 C25 1.338(6) . ?
N3 C33 1.435(6) . ?
N3 H3N 0.88(2) . ?
C1 C6 1.417(7) . ?
C1 C2 1.426(6) . ?
C1 C7 1.514(6) . ?
C2 C3 1.398(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.434(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.411(6) . ?
C4 C8 1.517(6) . ?
C5 C6 1.419(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.522(7) . ?
C8 C10 1.536(7) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.524(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C18 1.381(6) . ?
C13 C14 1.383(7) . ?
C14 C15 1.398(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.378(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.385(8) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.381(6) . ?
C19 C20 1.393(6) . ?
C20 C21 1.389(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.374(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.381(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.400(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C26 C27 1.364(9) . ?
C26 C31 1.381(8) . ?
C27 C28 1.391(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.383(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.378(9) . ?
C29 C32 1.507(7) . ?
C30 C31 1.384(7) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.378(6) . ?
C33 C38 1.411(7) . ?
C34 C35 1.393(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.386(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.391(6) . ?
C36 C39 1.501(6) . ?
C37 C38 1.376(7) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
Os51 C55 2.189(4) . ?
Os51 C56 2.191(4) . ?
Os51 C54 2.212(4) . ?
Os51 C51 2.213(4) . ?
Os51 C53 2.232(4) . ?
Os51 C52 2.235(4) . ?
Os51 P51 2.3611(11) . ?
Os51 Cl51 2.4187(10) . ?
Os51 Cl52 2.4302(10) . ?
P51 C63 1.819(4) . ?
P51 C69 1.826(4) . ?
P51 C61 1.851(4) . ?
N51 C75 1.326(5) . ?
N51 C62 1.457(5) . ?
N51 H51N 0.8742 . ?
N52 C75 1.339(5) . ?
N52 C76 1.424(5) . ?
N52 H52N 0.865(19) . ?
N53 C75 1.351(5) . ?
N53 C83 1.437(5) . ?
N53 H53N 0.858(19) . ?
C51 C56 1.421(7) . ?
C51 C52 1.431(7) . ?
C51 C57 1.512(6) . ?
C52 C53 1.390(7) . ?
C52 H52 0.9500 . ?
C53 C54 1.448(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.407(6) . ?
C54 C58 1.512(6) . ?
C55 C56 1.433(6) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C60 1.522(6) . ?
C58 C59 1.532(6) . ?
C58 H58 1.0000 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.533(5) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C68 1.393(6) . ?
C63 C64 1.398(6) . ?
C64 C65 1.389(6) . ?
C64 H64 0.9500 . ?
C65 C66 1.388(7) . ?
C65 H65 0.9500 . ?
C66 C67 1.381(7) . ?
C66 H66 0.9500 . ?
C67 C68 1.395(6) . ?
C67 H67 0.9500 . ?
C68 H68 0.9500 . ?
C69 C70 1.397(6) . ?
C69 C74 1.398(6) . ?
C70 C71 1.384(7) . ?
C70 H70 0.9500 . ?
C71 C72 1.390(8) . ?
C71 H71 0.9500 . ?
C72 C73 1.372(8) . ?
C72 H72 0.9500 . ?
C73 C74 1.384(7) . ?
C73 H73 0.9500 . ?
C74 H74 0.9500 . ?
C76 C81 1.373(6) . ?
C76 C77 1.398(6) . ?
C77 C78 1.376(6) . ?
C77 H77 0.9500 . ?
C78 C79 1.402(6) . ?
C78 H78 0.9500 . ?
C79 C80 1.385(6) . ?
C79 C82 1.508(6) . ?
C80 C81 1.387(6) . ?
C80 H80 0.9500 . ?
C81 H81 0.9500 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 C84 1.388(6) . ?
C83 C88 1.390(6) . ?
C84 C85 1.396(6) . ?
C84 H84 0.9500 . ?
C85 C86 1.399(7) . ?
C85 H85 0.9500 . ?
C86 C87 1.379(6) . ?
C86 C89 1.502(6) . ?
C87 C88 1.390(6) . ?
C87 H87 0.9500 . ?
C88 H88 0.9500 . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
Sb1 F3 1.856(3) . ?
Sb1 F2 1.864(3) . ?
Sb1 F6 1.868(3) . ?
Sb1 F5 1.873(3) . ?
Sb1 F4 1.876(3) . ?
Sb1 F1 1.886(3) . ?
Sb2 F11 1.865(3) . ?
Sb2 F9 1.870(3) . ?
Sb2 F10 1.872(3) . ?
Sb2 F8 1.874(3) . ?
Sb2 F12 1.874(3) . ?
Sb2 F7 1.876(3) . ?
C41 Cl4 1.745(6) . ?
C41 Cl3 1.765(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 Cl5B 1.726(7) . ?
C42 Cl6 1.760(7) . ?
C42 Cl5A 1.770(8) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 H42C 0.9900 . ?
C42 H42D 0.9900 . ?
C45 C46 1.533(11) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.492(10) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.487(11) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49A 1.59(2) . ?
C48 C49B 1.621(18) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 H48C 0.9900 . ?
C48 H48D 0.9900 . ?
C49A C50A 1.653(17) . ?
C49A H49A 0.9900 . ?
C49A H49B 0.9900 . ?
C50A H50A 0.9800 . ?
C50A H50B 0.9800 . ?
C50A H50C 0.9800 . ?
C49B C50B 1.76(3) . ?
C49B H49C 0.9900 . ?
C49B H49D 0.9900 . ?
C50B H50D 0.9800 . ?
C50B H50E 0.9800 . ?
C50B H50F 0.9800 . ?
C95 C96 1.432(14) . ?
C95 C95 1.486(19) 2_675 ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C96 C97 1.463(14) . ?
C96 H96A 0.9900 . ?
C96 H96B 0.9900 . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 Os1 C5 37.97(17) . . ?
C6 Os1 C1 37.79(18) . . ?
C5 Os1 C1 68.55(17) . . ?
C6 Os1 C2 67.25(17) . . ?
C5 Os1 C2 79.52(17) . . ?
C1 Os1 C2 37.59(17) . . ?
C6 Os1 C4 67.88(17) . . ?
C5 Os1 C4 37.25(16) . . ?
C1 Os1 C4 80.87(17) . . ?
C2 Os1 C4 67.28(17) . . ?
C6 Os1 C3 79.16(17) . . ?
C5 Os1 C3 66.97(16) . . ?
C1 Os1 C3 67.28(17) . . ?
C2 Os1 C3 36.54(16) . . ?
C4 Os1 C3 37.49(16) . . ?
C6 Os1 P1 92.28(12) . . ?
C5 Os1 P1 94.73(12) . . ?
C1 Os1 P1 116.27(12) . . ?
C2 Os1 P1 153.54(12) . . ?
C4 Os1 P1 121.86(12) . . ?
C3 Os1 P1 159.35(12) . . ?
C6 Os1 Cl1 122.43(13) . . ?
C5 Os1 Cl1 159.90(12) . . ?
C1 Os1 Cl1 91.86(14) . . ?
C2 Os1 Cl1 87.64(13) . . ?
C4 Os1 Cl1 147.42(12) . . ?
C3 Os1 Cl1 110.58(12) . . ?
P1 Os1 Cl1 89.90(4) . . ?
C6 Os1 Cl2 152.28(13) . . ?
C5 Os1 Cl2 114.47(12) . . ?
C1 Os1 Cl2 156.91(13) . . ?
C2 Os1 Cl2 119.32(12) . . ?
C4 Os1 Cl2 89.24(11) . . ?
C3 Os1 Cl2 92.27(12) . . ?
P1 Os1 Cl2 86.67(3) . . ?
Cl1 Os1 Cl2 85.29(4) . . ?
C19 P1 C13 102.75(19) . . ?
C19 P1 C11 101.23(19) . . ?
C13 P1 C11 103.4(2) . . ?
C19 P1 Os1 118.15(14) . . ?
C13 P1 Os1 112.02(14) . . ?
C11 P1 Os1 117.21(14) . . ?
C25 N1 C12 125.3(4) . . ?
C25 N1 H1N 112(4) . . ?
C12 N1 H1N 118(4) . . ?
C25 N2 C26 125.5(4) . . ?
C25 N2 H2N 118(4) . . ?
C26 N2 H2N 116(4) . . ?
C25 N3 C33 122.5(4) . . ?
C25 N3 H3N 116(4) . . ?
C33 N3 H3N 121(4) . . ?
C6 C1 C2 117.4(4) . . ?
C6 C1 C7 123.0(4) . . ?
C2 C1 C7 119.5(4) . . ?
C6 C1 Os1 69.6(2) . . ?
C2 C1 Os1 71.7(3) . . ?
C7 C1 Os1 130.3(4) . . ?
C3 C2 C1 121.4(4) . . ?
C3 C2 Os1 72.5(3) . . ?
C1 C2 Os1 70.7(2) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
Os1 C2 H2 130.1 . . ?
C2 C3 C4 120.7(4) . . ?
C2 C3 Os1 71.0(3) . . ?
C4 C3 Os1 70.7(2) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
Os1 C3 H3 131.6 . . ?
C5 C4 C3 118.5(4) . . ?
C5 C4 C8 122.8(4) . . ?
C3 C4 C8 118.7(4) . . ?
C5 C4 Os1 70.2(3) . . ?
C3 C4 Os1 71.8(3) . . ?
C8 C4 Os1 131.3(3) . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 Os1 72.6(3) . . ?
C6 C5 Os1 70.1(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
Os1 C5 H5 129.9 . . ?
C1 C6 C5 121.7(4) . . ?
C1 C6 Os1 72.6(3) . . ?
C5 C6 Os1 71.9(3) . . ?
C1 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
Os1 C6 H6 128.8 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 C9 114.8(4) . . ?
C4 C8 C10 108.2(4) . . ?
C9 C8 C10 111.0(4) . . ?
C4 C8 H8 107.5 . . ?
C9 C8 H8 107.5 . . ?
C10 C8 H8 107.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 P1 112.7(3) . . ?
C12 C11 H11A 109.1 . . ?
P1 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
P1 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
N1 C12 C11 110.8(4) . . ?
N1 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C18 C13 C14 119.2(4) . . ?
C18 C13 P1 120.2(4) . . ?
C14 C13 P1 120.6(3) . . ?
C13 C14 C15 120.6(5) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C16 C15 C14 119.8(5) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 119.6(5) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 120.4(5) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C13 C18 C17 120.5(5) . . ?
C13 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C24 C19 C20 119.7(4) . . ?
C24 C19 P1 121.5(3) . . ?
C20 C19 P1 118.6(3) . . ?
C21 C20 C19 119.5(4) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C22 C21 C20 120.8(4) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C23 120.2(4) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C24 119.5(5) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C19 C24 C23 120.4(4) . . ?
C19 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
N1 C25 N3 120.2(4) . . ?
N1 C25 N2 120.0(4) . . ?
N3 C25 N2 119.8(5) . . ?
C27 C26 C31 120.7(5) . . ?
C27 C26 N2 118.4(5) . . ?
C31 C26 N2 120.8(6) . . ?
C26 C27 C28 119.4(6) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C29 C28 C27 121.3(6) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C30 C29 C28 117.8(5) . . ?
C30 C29 C32 121.7(6) . . ?
C28 C29 C32 120.6(6) . . ?
C29 C30 C31 121.9(6) . . ?
C29 C30 H30 119.1 . . ?
C31 C30 H30 119.1 . . ?
C26 C31 C30 118.9(6) . . ?
C26 C31 H31 120.6 . . ?
C30 C31 H31 120.6 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C38 120.3(4) . . ?
C34 C33 N3 120.1(4) . . ?
C38 C33 N3 119.6(4) . . ?
C33 C34 C35 119.5(4) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C36 C35 C34 121.1(4) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C35 C36 C37 118.3(4) . . ?
C35 C36 C39 120.4(4) . . ?
C37 C36 C39 121.2(4) . . ?
C38 C37 C36 121.9(4) . . ?
C38 C37 H37 119.0 . . ?
C36 C37 H37 119.0 . . ?
C37 C38 C33 118.6(4) . . ?
C37 C38 H38 120.7 . . ?
C33 C38 H38 120.7 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C55 Os51 C56 38.21(15) . . ?
C55 Os51 C54 37.27(15) . . ?
C56 Os51 C54 68.39(16) . . ?
C55 Os51 C51 68.43(16) . . ?
C56 Os51 C51 37.64(17) . . ?
C54 Os51 C51 81.17(16) . . ?
C55 Os51 C53 67.12(16) . . ?
C56 Os51 C53 79.41(17) . . ?
C54 Os51 C53 38.03(15) . . ?
C51 Os51 C53 67.09(17) . . ?
C55 Os51 C52 79.34(16) . . ?
C56 Os51 C52 67.20(17) . . ?
C54 Os51 C52 67.57(16) . . ?
C51 Os51 C52 37.51(18) . . ?
C53 Os51 C52 36.27(17) . . ?
C55 Os51 P51 94.69(11) . . ?
C56 Os51 P51 94.71(12) . . ?
C54 Os51 P51 119.47(11) . . ?
C51 Os51 P51 120.21(14) . . ?
C53 Os51 P51 157.34(12) . . ?
C52 Os51 P51 157.57(14) . . ?
C55 Os51 Cl51 155.63(11) . . ?
C56 Os51 Cl51 117.42(12) . . ?
C54 Os51 Cl51 153.42(11) . . ?
C51 Os51 Cl51 89.85(12) . . ?
C53 Os51 Cl51 115.55(12) . . ?
C52 Os51 Cl51 90.16(12) . . ?
P51 Os51 Cl51 86.67(4) . . ?
C55 Os51 Cl52 118.07(11) . . ?
C56 Os51 Cl52 156.27(12) . . ?
C54 Os51 Cl52 90.85(11) . . ?
C51 Os51 Cl52 153.83(14) . . ?
C53 Os51 Cl52 91.36(12) . . ?
C52 Os51 Cl52 116.54(13) . . ?
P51 Os51 Cl52 85.43(3) . . ?
Cl51 Os51 Cl52 86.30(4) . . ?
C63 P51 C69 103.96(19) . . ?
C63 P51 C61 103.56(18) . . ?
C69 P51 C61 101.11(19) . . ?
C63 P51 Os51 113.24(13) . . ?
C69 P51 Os51 116.69(15) . . ?
C61 P51 Os51 116.48(14) . . ?
C75 N51 C62 124.1(3) . . ?
C75 N51 H51N 116.4 . . ?
C62 N51 H51N 118.9 . . ?
C75 N52 C76 127.6(3) . . ?
C75 N52 H52N 114(3) . . ?
C76 N52 H52N 118(3) . . ?
C75 N53 C83 123.1(3) . . ?
C75 N53 H53N 113(3) . . ?
C83 N53 H53N 122(3) . . ?
C56 C51 C52 118.4(4) . . ?
C56 C51 C57 121.7(5) . . ?
C52 C51 C57 119.8(4) . . ?
C56 C51 Os51 70.3(2) . . ?
C52 C51 Os51 72.1(2) . . ?
C57 C51 Os51 130.4(3) . . ?
C53 C52 C51 121.1(4) . . ?
C53 C52 Os51 71.7(2) . . ?
C51 C52 Os51 70.4(2) . . ?
C53 C52 H52 119.5 . . ?
C51 C52 H52 119.5 . . ?
Os51 C52 H52 131.3 . . ?
C52 C53 C54 121.2(4) . . ?
C52 C53 Os51 72.0(3) . . ?
C54 C53 Os51 70.3(2) . . ?
C52 C53 H53 119.4 . . ?
C54 C53 H53 119.4 . . ?
Os51 C53 H53 131.2 . . ?
C55 C54 C53 117.8(4) . . ?
C55 C54 C58 123.0(4) . . ?
C53 C54 C58 119.0(4) . . ?
C55 C54 Os51 70.5(2) . . ?
C53 C54 Os51 71.7(2) . . ?
C58 C54 Os51 133.4(3) . . ?
C54 C55 C56 121.2(4) . . ?
C54 C55 Os51 72.3(2) . . ?
C56 C55 Os51 71.0(2) . . ?
C54 C55 H55 119.4 . . ?
C56 C55 H55 119.4 . . ?
Os51 C55 H55 130.0 . . ?
C51 C56 C55 120.3(4) . . ?
C51 C56 Os51 72.0(2) . . ?
C55 C56 Os51 70.8(2) . . ?
C51 C56 H56 119.9 . . ?
C55 C56 H56 119.9 . . ?
Os51 C56 H56 129.7 . . ?
C51 C57 H57A 109.5 . . ?
C51 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C51 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C54 C58 C60 114.3(4) . . ?
C54 C58 C59 107.9(3) . . ?
C60 C58 C59 111.5(4) . . ?
C54 C58 H58 107.7 . . ?
C60 C58 H58 107.7 . . ?
C59 C58 H58 107.7 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 P51 114.0(3) . . ?
C62 C61 H61A 108.8 . . ?
P51 C61 H61A 108.8 . . ?
C62 C61 H61B 108.8 . . ?
P51 C61 H61B 108.8 . . ?
H61A C61 H61B 107.7 . . ?
N51 C62 C61 111.4(3) . . ?
N51 C62 H62A 109.4 . . ?
C61 C62 H62A 109.4 . . ?
N51 C62 H62B 109.4 . . ?
C61 C62 H62B 109.4 . . ?
H62A C62 H62B 108.0 . . ?
C68 C63 C64 119.2(4) . . ?
C68 C63 P51 120.7(3) . . ?
C64 C63 P51 120.0(3) . . ?
C65 C64 C63 120.3(4) . . ?
C65 C64 H64 119.9 . . ?
C63 C64 H64 119.9 . . ?
C66 C65 C64 119.9(4) . . ?
C66 C65 H65 120.1 . . ?
C64 C65 H65 120.1 . . ?
C67 C66 C65 120.6(4) . . ?
C67 C66 H66 119.7 . . ?
C65 C66 H66 119.7 . . ?
C66 C67 C68 119.6(4) . . ?
C66 C67 H67 120.2 . . ?
C68 C67 H67 120.2 . . ?
C63 C68 C67 120.5(4) . . ?
C63 C68 H68 119.7 . . ?
C67 C68 H68 119.7 . . ?
C70 C69 C74 119.5(4) . . ?
C70 C69 P51 121.0(3) . . ?
C74 C69 P51 118.8(3) . . ?
C71 C70 C69 119.8(5) . . ?
C71 C70 H70 120.1 . . ?
C69 C70 H70 120.1 . . ?
C70 C71 C72 120.5(5) . . ?
C70 C71 H71 119.8 . . ?
C72 C71 H71 119.8 . . ?
C73 C72 C71 119.6(5) . . ?
C73 C72 H72 120.2 . . ?
C71 C72 H72 120.2 . . ?
C72 C73 C74 121.0(5) . . ?
C72 C73 H73 119.5 . . ?
C74 C73 H73 119.5 . . ?
C73 C74 C69 119.6(5) . . ?
C73 C74 H74 120.2 . . ?
C69 C74 H74 120.2 . . ?
N51 C75 N52 119.5(4) . . ?
N51 C75 N53 120.6(4) . . ?
N52 C75 N53 119.9(4) . . ?
C81 C76 C77 120.1(4) . . ?
C81 C76 N52 122.9(4) . . ?
C77 C76 N52 116.8(4) . . ?
C78 C77 C76 120.3(4) . . ?
C78 C77 H77 119.9 . . ?
C76 C77 H77 119.9 . . ?
C77 C78 C79 120.5(4) . . ?
C77 C78 H78 119.8 . . ?
C79 C78 H78 119.8 . . ?
C80 C79 C78 117.8(4) . . ?
C80 C79 C82 122.5(4) . . ?
C78 C79 C82 119.7(4) . . ?
C79 C80 C81 122.3(4) . . ?
C79 C80 H80 118.9 . . ?
C81 C80 H80 118.9 . . ?
C76 C81 C80 119.0(4) . . ?
C76 C81 H81 120.5 . . ?
C80 C81 H81 120.5 . . ?
C79 C82 H82A 109.5 . . ?
C79 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C79 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C84 C83 C88 120.3(4) . . ?
C84 C83 N53 119.4(4) . . ?
C88 C83 N53 120.2(4) . . ?
C83 C84 C85 118.8(4) . . ?
C83 C84 H84 120.6 . . ?
C85 C84 H84 120.6 . . ?
C84 C85 C86 121.7(4) . . ?
C84 C85 H85 119.1 . . ?
C86 C85 H85 119.1 . . ?
C87 C86 C85 118.0(4) . . ?
C87 C86 C89 120.8(4) . . ?
C85 C86 C89 121.3(4) . . ?
C86 C87 C88 121.5(4) . . ?
C86 C87 H87 119.2 . . ?
C88 C87 H87 119.2 . . ?
C87 C88 C83 119.6(4) . . ?
C87 C88 H88 120.2 . . ?
C83 C88 H88 120.2 . . ?
C86 C89 H89A 109.5 . . ?
C86 C89 H89B 109.5 . . ?
H89A C89 H89B 109.5 . . ?
C86 C89 H89C 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
F3 Sb1 F2 90.44(15) . . ?
F3 Sb1 F6 91.0(2) . . ?
F2 Sb1 F6 90.12(16) . . ?
F3 Sb1 F5 91.65(18) . . ?
F2 Sb1 F5 89.86(14) . . ?
F6 Sb1 F5 177.39(19) . . ?
F3 Sb1 F4 177.39(17) . . ?
F2 Sb1 F4 91.35(15) . . ?
F6 Sb1 F4 87.13(19) . . ?
F5 Sb1 F4 90.26(17) . . ?
F3 Sb1 F1 89.77(16) . . ?
F2 Sb1 F1 179.46(16) . . ?
F6 Sb1 F1 90.38(16) . . ?
F5 Sb1 F1 89.64(15) . . ?
F4 Sb1 F1 88.45(15) . . ?
F11 Sb2 F9 89.94(13) . . ?
F11 Sb2 F10 90.17(13) . . ?
F9 Sb2 F10 179.30(16) . . ?
F11 Sb2 F8 91.04(13) . . ?
F9 Sb2 F8 91.19(16) . . ?
F10 Sb2 F8 89.50(15) . . ?
F11 Sb2 F12 179.41(14) . . ?
F9 Sb2 F12 90.64(13) . . ?
F10 Sb2 F12 89.25(13) . . ?
F8 Sb2 F12 89.02(15) . . ?
F11 Sb2 F7 91.23(13) . . ?
F9 Sb2 F7 88.81(15) . . ?
F10 Sb2 F7 90.50(14) . . ?
F8 Sb2 F7 177.73(13) . . ?
F12 Sb2 F7 88.71(14) . . ?
Cl4 C41 Cl3 111.9(3) . . ?
Cl4 C41 H41A 109.2 . . ?
Cl3 C41 H41A 109.2 . . ?
Cl4 C41 H41B 109.2 . . ?
Cl3 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
Cl5B C42 Cl6 112.6(4) . . ?
Cl6 C42 Cl5A 111.2(4) . . ?
Cl6 C42 H42A 109.4 . . ?
Cl5A C42 H42A 109.4 . . ?
Cl6 C42 H42B 109.4 . . ?
Cl5A C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?
Cl5B C42 H42C 109.1 . . ?
Cl6 C42 H42C 109.1 . . ?
Cl5B C42 H42D 109.1 . . ?
Cl6 C42 H42D 109.1 . . ?
H42C C42 H42D 107.8 . . ?
C46 C45 H45A 109.5 . . ?
C46 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C46 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 C45 113.5(6) . . ?
C47 C46 H46A 108.9 . . ?
C45 C46 H46A 108.9 . . ?
C47 C46 H46B 108.9 . . ?
C45 C46 H46B 108.9 . . ?
H46A C46 H46B 107.7 . . ?
C48 C47 C46 115.1(7) . . ?
C48 C47 H47A 108.5 . . ?
C46 C47 H47A 108.5 . . ?
C48 C47 H47B 108.5 . . ?
C46 C47 H47B 108.5 . . ?
H47A C47 H47B 107.5 . . ?
C47 C48 C49A 119.2(10) . . ?
C47 C48 C49B 114.5(9) . . ?
C47 C48 H48A 107.5 . . ?
C49A C48 H48A 107.5 . . ?
C47 C48 H48B 107.5 . . ?
C49A C48 H48B 107.5 . . ?
H48A C48 H48B 107.0 . . ?
C47 C48 H48C 108.6 . . ?
C49B C48 H48C 108.6 . . ?
C47 C48 H48D 108.6 . . ?
C49B C48 H48D 108.6 . . ?
H48C C48 H48D 107.6 . . ?
C48 C49A C50A 100.7(14) . . ?
C48 C49A H49A 111.6 . . ?
C50A C49A H49A 111.6 . . ?
C48 C49A H49B 111.6 . . ?
C50A C49A H49B 111.6 . . ?
H49A C49A H49B 109.4 . . ?
C49A C50A H50A 109.5 . . ?
C49A C50A H50B 109.5 . . ?
H50A C50A H50B 109.5 . . ?
C49A C50A H50C 109.5 . . ?
H50A C50A H50C 109.5 . . ?
H50B C50A H50C 109.5 . . ?
C48 C49B C50B 95.9(13) . . ?
C48 C49B H49C 112.6 . . ?
C50B C49B H49C 112.6 . . ?
C48 C49B H49D 112.6 . . ?
C50B C49B H49D 112.6 . . ?
H49C C49B H49D 110.1 . . ?
C49B C50B H50D 109.5 . . ?
C49B C50B H50E 109.5 . . ?
H50D C50B H50E 109.5 . . ?
C49B C50B H50F 109.5 . . ?
H50D C50B H50F 109.5 . . ?
H50E C50B H50F 109.5 . . ?
C96 C95 C95 125.1(14) . 2_675 ?
C96 C95 H95A 106.0 . . ?
C95 C95 H95A 106.0 2_675 . ?
C96 C95 H95B 106.0 . . ?
C95 C95 H95B 106.0 2_675 . ?
H95A C95 H95B 106.3 . . ?
C95 C96 C97 118.0(12) . . ?
C95 C96 H96A 107.8 . . ?
C97 C96 H96A 107.8 . . ?
C95 C96 H96B 107.8 . . ?
C97 C96 H96B 107.8 . . ?
H96A C96 H96B 107.2 . . ?
C96 C97 H97A 109.5 . . ?
C96 C97 H97B 109.5 . . ?
H97A C97 H97B 109.5 . . ?
C96 C97 H97C 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?

_refine_diff_density_max         2.620
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.131

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/hexane'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cmpnd_4
_database_code_depnum_ccdc_archive 'CCDC 1983333'
loop_
_audit_author_name
_audit_author_address
'Pilar Garcia-Orduna'
;Instituto de Sintesis Quimica y Catalisis Homogenea (ISQCH, CSIC Univ Zaragoza)
Spain
;
_audit_update_record             
;
2020-07-31 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H38 N4 O Os, 2(F6 Sb), 2(C H2 Cl2)'
_chemical_formula_sum            'C33 H42 Cl4 F12 N4 O Os Sb2'
_chemical_formula_weight         1314.20

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'
H H 0.0000 0.0000 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.709(8)
_cell_length_b                   15.2562(14)
_cell_length_c                   17.6428(16)
_cell_angle_alpha                110.1590(10)
_cell_angle_beta                 92.3050(10)
_cell_angle_gamma                98.7480(10)
_cell_volume                     2164(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4367
_cell_measurement_theta_min      2.378
_cell_measurement_theta_max      27.970

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_F_000             1260
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    4.499
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4359
_exptl_absorpt_correction_T_max  0.6240
_exptl_absorpt_process_details   
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.

;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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 APEX CCD system'
_diffrn_measurement_method       'narrow ω frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_decay_%        0
_diffrn_reflns_number            22268
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.210
_diffrn_reflns_theta_max         28.156
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             9848
_reflns_number_gt                6988
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_cell_refinement       'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'

_refine_special_details          
;
The asymmetric unit is formed by an osmium complex, two SbF6 counterions and two
dichloromethane solvent molecules.

Four low angle reflections (1 0 0 ,0 1 0,0 0 1 and 0 -1 0) have been found to be
affected by the beamstop. They have been excluded during the data refinement.

Four fluorine atoms of a counterion have been found to be disordered. They have
been included in the model in two sets of positions with complementary 
occupancy factors (0.60/0.40(2)) and isotropically refined.

In order to increase the data/parameters ratio, most of the hydrogen atoms (except 
those of N-H and coordinated water group)have been included in the model in 
calculated positions and refined with a riding model.

Hydrogen atoms of NH groups have been observed in Fourier difference maps, included 
in the model in observed positions and refined with a restraint in N-H bond length.
The refinement of their isotropic atomic displacement parameter leads to a NPD value
in the case of H3N. Therefore, its Uiso has been restrained to be equal to -1.2 times
Ueq of N3.

Hydrogen atoms of coordinated water have not been observed in Fourier difference maps.
HFIX 137 instruction have been used to calculate their possible positions. Afterwards, 
the geometrical restraint has been relaxed. The "three hydrogen atoms" have been 
refined with a restrain in O-H bond length. The value of their obtained Uiso value
have been used as criteria to select the two most suitable positions. 

At the end of the refinement, when convergence is achieved, residual density peaks are
observed close to heaviest atoms (Os and Sb). They have no chemical sense.

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0486P)²+10.8565P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Direct method'
_atom_sites_solution_secondary   'Fourier Difference Synthesis'
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9848
_refine_ls_number_parameters     531
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0636
_refine_ls_wR_factor_ref         0.1383
_refine_ls_wR_factor_gt          0.1225
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.73024(4) 0.87424(3) 0.68078(2) 0.01902(11) Uani 1 1 d . . . . .
O O 0.9402(8) 0.8120(5) 0.6745(4) 0.0230(14) Uani 1 1 d D . . . .
N1 N 0.8846(9) 0.9981(6) 0.7430(5) 0.0235(18) Uani 1 1 d . . . . .
N2 N 0.7568(8) 0.8710(5) 0.7980(4) 0.0174(16) Uani 1 1 d . . . . .
N3 N 0.7241(10) 0.7095(6) 0.7629(5) 0.0228(17) Uani 1 1 d D . . . .
H3N H 0.780(10) 0.713(7) 0.724(4) 0.027 Uiso 1 1 d D U . . .
N4 N 0.6955(9) 0.8059(6) 0.8969(4) 0.0199(16) Uani 1 1 d D . . . .
C1 C 0.6001(12) 0.7545(8) 0.5787(6) 0.029(2) Uani 1 1 d . . . . .
C2 C 0.5055(11) 0.7809(7) 0.6390(6) 0.026(2) Uani 1 1 d . . . . .
H2 H 0.4524 0.7334 0.6566 0.031 Uiso 1 1 calc R U . . .
C3 C 0.4820(11) 0.8747(7) 0.6768(6) 0.024(2) Uani 1 1 d . . . . .
H3 H 0.4181 0.8894 0.7203 0.029 Uiso 1 1 calc R U . . .
C4 C 0.5540(10) 0.9483(7) 0.6498(6) 0.022(2) Uani 1 1 d . . . . .
C5 C 0.6462(11) 0.9206(8) 0.5836(6) 0.027(2) Uani 1 1 d . . . . .
H5 H 0.6928 0.9668 0.5627 0.032 Uiso 1 1 calc R U . . .
C6 C 0.6699(11) 0.8260(8) 0.5483(6) 0.030(2) Uani 1 1 d . . . . .
H6 H 0.7323 0.8095 0.5042 0.036 Uiso 1 1 calc R U . . .
C7 C 0.6332(13) 0.6561(8) 0.5411(7) 0.039(3) Uani 1 1 d . . . . .
H7A H 0.6062 0.6205 0.5769 0.058 Uiso 1 1 calc R U . . .
H7B H 0.7443 0.6591 0.5332 0.058 Uiso 1 1 calc R U . . .
H7C H 0.5707 0.6244 0.4885 0.058 Uiso 1 1 calc R U . . .
C8 C 0.5369(12) 1.0505(7) 0.6889(6) 0.029(2) Uani 1 1 d . . . . .
H8 H 0.6410 1.0901 0.6918 0.035 Uiso 1 1 calc R U . . .
C9 C 0.4247(13) 1.0737(8) 0.6341(6) 0.035(3) Uani 1 1 d . . . . .
H9A H 0.4626 1.0600 0.5804 0.053 Uiso 1 1 calc R U . . .
H9B H 0.4173 1.1410 0.6573 0.053 Uiso 1 1 calc R U . . .
H9C H 0.3215 1.0350 0.6290 0.053 Uiso 1 1 calc R U . . .
C10 C 0.4901(14) 1.0763(8) 0.7749(6) 0.038(3) Uani 1 1 d . . . . .
H10A H 0.3910 1.0361 0.7749 0.057 Uiso 1 1 calc R U . . .
H10B H 0.4779 1.1431 0.7955 0.057 Uiso 1 1 calc R U . . .
H10C H 0.5712 1.0665 0.8098 0.057 Uiso 1 1 calc R U . . .
C11 C 0.9716(10) 1.0518(7) 0.7077(6) 0.024(2) Uani 1 1 d . . . . .
H11 H 0.9649 1.0303 0.6501 0.029 Uiso 1 1 calc R U . . .
C12 C 1.0696(11) 1.1361(8) 0.7512(7) 0.031(2) Uani 1 1 d . . . . .
H12 H 1.1271 1.1729 0.7245 0.037 Uiso 1 1 calc R U . . .
C13 C 1.0810(12) 1.1653(8) 0.8350(7) 0.031(2) Uani 1 1 d . . . . .
H13 H 1.1483 1.2225 0.8669 0.037 Uiso 1 1 calc R U . . .
C14 C 0.9945(12) 1.1109(7) 0.8721(6) 0.030(2) Uani 1 1 d . . . . .
H14 H 1.0015 1.1303 0.9296 0.036 Uiso 1 1 calc R U . . .
C15 C 0.8977(10) 1.0278(7) 0.8244(6) 0.021(2) Uani 1 1 d . . . . .
C16 C 0.8013(12) 0.9666(7) 0.8614(6) 0.025(2) Uani 1 1 d . . . . .
H16A H 0.8622 0.9631 0.9086 0.030 Uiso 1 1 calc R U . . .
H16B H 0.7068 0.9931 0.8801 0.030 Uiso 1 1 calc R U . . .
C17 C 0.7237(10) 0.7963(7) 0.8192(6) 0.022(2) Uani 1 1 d . . . . .
C18 C 0.6218(11) 0.6229(7) 0.7505(6) 0.022(2) Uani 1 1 d . . . . .
C19 C 0.6641(12) 0.5392(7) 0.7017(6) 0.030(2) Uani 1 1 d . . . . .
H19 H 0.7606 0.5411 0.6785 0.036 Uiso 1 1 calc R U . . .
C20 C 0.5685(12) 0.4536(7) 0.6863(6) 0.030(2) Uani 1 1 d . . . . .
H20 H 0.5980 0.3975 0.6508 0.036 Uiso 1 1 calc R U . . .
C21 C 0.4269(13) 0.4471(8) 0.7221(7) 0.034(3) Uani 1 1 d . . . . .
C22 C 0.3893(11) 0.5312(8) 0.7700(6) 0.028(2) Uani 1 1 d . . . . .
H22 H 0.2946 0.5294 0.7947 0.033 Uiso 1 1 calc R U . . .
C23 C 0.4807(11) 0.6185(7) 0.7845(6) 0.026(2) Uani 1 1 d . . . . .
H23 H 0.4479 0.6749 0.8173 0.031 Uiso 1 1 calc R U . . .
C24 C 0.3311(15) 0.3526(9) 0.7082(9) 0.054(4) Uani 1 1 d . . . . .
H24A H 0.3658 0.3280 0.7493 0.080 Uiso 1 1 calc R U . . .
H24B H 0.3433 0.3087 0.6541 0.080 Uiso 1 1 calc R U . . .
H24C H 0.2210 0.3587 0.7122 0.080 Uiso 1 1 calc R U . . .
C25 C 0.7040(11) 0.7395(7) 0.9356(6) 0.024(2) Uani 1 1 d . . . . .
C26 C 0.8205(11) 0.6832(7) 0.9232(6) 0.025(2) Uani 1 1 d . . . . .
H26 H 0.8981 0.6890 0.8880 0.031 Uiso 1 1 calc R U . . .
C27 C 0.8212(12) 0.6194(7) 0.9625(6) 0.029(2) Uani 1 1 d . . . . .
H27 H 0.8986 0.5802 0.9527 0.034 Uiso 1 1 calc R U . . .
C28 C 0.7116(13) 0.6105(8) 1.0162(6) 0.032(3) Uani 1 1 d . . . . .
C29 C 0.5982(12) 0.6673(8) 1.0280(7) 0.035(3) Uani 1 1 d . . . . .
H29 H 0.5219 0.6626 1.0640 0.042 Uiso 1 1 calc R U . . .
C30 C 0.5947(11) 0.7309(7) 0.9877(6) 0.027(2) Uani 1 1 d . . . . .
H30 H 0.5157 0.7690 0.9964 0.032 Uiso 1 1 calc R U . . .
C31 C 0.7152(15) 0.5421(8) 1.0608(7) 0.044(3) Uani 1 1 d . . . . .
H31A H 0.7802 0.5740 1.1126 0.066 Uiso 1 1 calc R U . . .
H31B H 0.7588 0.4874 1.0278 0.066 Uiso 1 1 calc R U . . .
H31C H 0.6088 0.5205 1.0710 0.066 Uiso 1 1 calc R U . . .
Sb1 Sb 0.75551(7) 0.11011(5) 0.09632(4) 0.02318(16) Uani 1 1 d . . . . .
F1 F 0.6644(7) 0.1210(5) 0.0029(4) 0.0378(15) Uani 1 1 d . . . . .
F2 F 0.8456(6) 0.1011(5) 0.1924(3) 0.0342(14) Uani 1 1 d . . . . .
F3 F 0.8015(9) 0.2404(5) 0.1435(4) 0.0535(19) Uani 1 1 d . . . . .
F4 F 0.7117(7) -0.0213(4) 0.0501(4) 0.0360(14) Uani 1 1 d . . . . .
F5 F 0.5646(7) 0.1105(5) 0.1402(4) 0.0401(16) Uani 1 1 d . . . . .
F6 F 0.9484(6) 0.1086(5) 0.0545(4) 0.0365(15) Uani 1 1 d . . . . .
Sb2 Sb 0.12985(8) 0.79281(5) 0.44926(5) 0.03193(18) Uani 1 1 d . . . . .
F7 F 0.1428(12) 0.7724(7) 0.3396(5) 0.087(3) Uani 1 1 d . . . . .
F8 F 0.1211(10) 0.8172(7) 0.5595(5) 0.078(3) Uani 1 1 d . . . . .
F9A F 0.2913(18) 0.9001(9) 0.4740(8) 0.044(4) Uiso 0.60(2) 1 d . . P A 1
F10A F -0.0346(16) 0.6976(9) 0.4418(9) 0.049(4) Uiso 0.60(2) 1 d . . P A 1
F11A F -0.0134(17) 0.8775(12) 0.4636(10) 0.058(4) Uiso 0.60(2) 1 d . . P A 1
F12A F 0.3094(17) 0.7404(11) 0.4571(8) 0.044(4) Uiso 0.60(2) 1 d . . P A 1
F9B F 0.232(4) 0.9085(19) 0.4672(17) 0.080(9) Uiso 0.40(2) 1 d . . P A 2
F10B F 0.019(3) 0.6695(16) 0.4098(15) 0.063(7) Uiso 0.40(2) 1 d . . P A 2
F11B F -0.053(2) 0.8352(15) 0.4300(13) 0.040(5) Uiso 0.40(2) 1 d . . P A 2
F12B F 0.260(2) 0.7082(14) 0.4401(11) 0.033(5) Uiso 0.40(2) 1 d . . P A 2
C51 C 0.1652(15) 0.5297(8) 0.5999(7) 0.043(3) Uani 1 1 d . . . . .
H51A H 0.2564 0.5106 0.6214 0.051 Uiso 1 1 calc R U . . .
H51B H 0.0795 0.4741 0.5815 0.051 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2147(4) 0.5621(2) 0.5172(2) 0.0493(8) Uani 1 1 d . . . . .
Cl2 Cl 0.1066(4) 0.6213(2) 0.6776(2) 0.0516(8) Uani 1 1 d . . . . .
C52 C 0.2172(15) 0.6108(11) 0.1903(9) 0.058(4) Uani 1 1 d . . . . .
H52A H 0.2688 0.6603 0.2414 0.070 Uiso 1 1 calc R U . . .
H52B H 0.2916 0.5677 0.1679 0.070 Uiso 1 1 calc R U . . .
Cl3 Cl 0.0478(4) 0.5451(3) 0.2120(2) 0.0692(11) Uani 1 1 d . . . . .
Cl4 Cl 0.1729(5) 0.6641(3) 0.1217(3) 0.0804(13) Uani 1 1 d . . . . .
H0A H 0.994(16) 0.792(11) 0.636(6) 0.10(6) Uiso 1 1 d D . . . .
H0B H 1.015(10) 0.834(8) 0.711(5) 0.05(4) Uiso 1 1 d D . . . .
H4N H 0.671(12) 0.860(4) 0.925(5) 0.03(3) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os N1 2.064(8) . ?
Os N2 2.090(7) . ?
Os C3 2.162(10) . ?
Os C2 2.171(10) . ?
Os O 2.174(7) . ?
Os C1 2.193(10) . ?
Os C4 2.195(8) . ?
Os C5 2.206(8) . ?
Os C6 2.209(9) . ?
O H0A 0.84(2) . ?
O H0B 0.84(2) . ?
N1 C15 1.341(11) . ?
N1 C11 1.355(11) . ?
N2 C17 1.313(11) . ?
N2 C16 1.483(12) . ?
N3 C17 1.356(13) . ?
N3 C18 1.419(12) . ?
N3 H3N 0.87(2) . ?
N4 C17 1.363(11) . ?
N4 C25 1.412(11) . ?
N4 H4N 0.87(2) . ?
C1 C2 1.360(14) . ?
C1 C6 1.442(14) . ?
C1 C7 1.495(15) . ?
C2 C3 1.406(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.435(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.423(13) . ?
C4 C8 1.505(13) . ?
C5 C6 1.412(14) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.510(12) . ?
C8 C10 1.519(14) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.380(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(14) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(14) . ?
C14 H14 0.9500 . ?
C15 C16 1.493(12) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 C19 1.386(14) . ?
C18 C23 1.391(14) . ?
C19 C20 1.371(14) . ?
C19 H19 0.9500 . ?
C20 C21 1.413(15) . ?
C20 H20 0.9500 . ?
C21 C22 1.367(15) . ?
C21 C24 1.487(15) . ?
C22 C23 1.377(14) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C30 1.373(13) . ?
C25 C26 1.404(14) . ?
C26 C27 1.376(13) . ?
C26 H26 0.9500 . ?
C27 C28 1.397(15) . ?
C27 H27 0.9500 . ?
C28 C29 1.385(16) . ?
C28 C31 1.511(13) . ?
C29 C30 1.389(13) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
Sb1 F3 1.842(7) . ?
Sb1 F4 1.856(6) . ?
Sb1 F6 1.862(6) . ?
Sb1 F5 1.862(6) . ?
Sb1 F1 1.871(5) . ?
Sb1 F2 1.896(5) . ?
Sb2 F9B 1.77(3) . ?
Sb2 F12B 1.816(16) . ?
Sb2 F10A 1.843(12) . ?
Sb2 F10B 1.86(2) . ?
Sb2 F8 1.857(7) . ?
Sb2 F7 1.862(8) . ?
Sb2 F11B 1.871(17) . ?
Sb2 F12A 1.882(13) . ?
Sb2 F11A 1.893(14) . ?
Sb2 F9A 1.899(13) . ?
C51 Cl1 1.745(12) . ?
C51 Cl2 1.745(12) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 Cl4 1.736(13) . ?
C52 Cl3 1.786(14) . ?
C52 H52A 0.9900 . ?
C52 H52B 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 Os N2 76.8(3) . . ?
N1 Os C3 119.7(3) . . ?
N2 Os C3 96.2(3) . . ?
N1 Os C2 157.2(3) . . ?
N2 Os C2 98.9(3) . . ?
C3 Os C2 37.9(4) . . ?
N1 Os O 82.7(3) . . ?
N2 Os O 79.7(3) . . ?
C3 Os O 156.0(3) . . ?
C2 Os O 118.9(3) . . ?
N1 Os C1 159.7(3) . . ?
N2 Os C1 122.5(3) . . ?
C3 Os C1 68.1(4) . . ?
C2 Os C1 36.3(4) . . ?
O Os C1 93.9(3) . . ?
N1 Os C4 93.7(3) . . ?
N2 Os C4 119.7(3) . . ?
C3 Os C4 38.4(3) . . ?
C2 Os C4 68.7(4) . . ?
O Os C4 159.1(3) . . ?
C1 Os C4 82.3(4) . . ?
N1 Os C5 96.2(3) . . ?
N2 Os C5 156.7(3) . . ?
C3 Os C5 67.7(4) . . ?
C2 Os C5 78.9(4) . . ?
O Os C5 121.9(3) . . ?
C1 Os C5 68.5(4) . . ?
C4 Os C5 37.7(3) . . ?
N1 Os C6 121.9(4) . . ?
N2 Os C6 160.3(3) . . ?
C3 Os C6 79.9(4) . . ?
C2 Os C6 66.2(4) . . ?
O Os C6 96.0(3) . . ?
C1 Os C6 38.2(4) . . ?
C4 Os C6 68.4(4) . . ?
C5 Os C6 37.3(4) . . ?
Os O H0A 131(10) . . ?
Os O H0B 122(9) . . ?
H0A O H0B 96(10) . . ?
C15 N1 C11 118.0(8) . . ?
C15 N1 Os 117.4(6) . . ?
C11 N1 Os 124.7(6) . . ?
C17 N2 C16 119.7(7) . . ?
C17 N2 Os 126.7(6) . . ?
C16 N2 Os 113.2(5) . . ?
C17 N3 C18 128.5(8) . . ?
C17 N3 H3N 112(7) . . ?
C18 N3 H3N 118(7) . . ?
C17 N4 C25 127.7(8) . . ?
C17 N4 H4N 114(7) . . ?
C25 N4 H4N 118(7) . . ?
C2 C1 C6 117.3(10) . . ?
C2 C1 C7 124.4(10) . . ?
C6 C1 C7 118.3(10) . . ?
C2 C1 Os 71.0(6) . . ?
C6 C1 Os 71.5(6) . . ?
C7 C1 Os 129.2(7) . . ?
C1 C2 C3 123.8(10) . . ?
C1 C2 Os 72.7(6) . . ?
C3 C2 Os 70.7(6) . . ?
C1 C2 H2 118.1 . . ?
C3 C2 H2 118.1 . . ?
Os C2 H2 131.7 . . ?
C2 C3 C4 120.2(9) . . ?
C2 C3 Os 71.4(6) . . ?
C4 C3 Os 72.0(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
Os C3 H3 129.0 . . ?
C5 C4 C3 116.6(9) . . ?
C5 C4 C8 120.5(9) . . ?
C3 C4 C8 122.9(9) . . ?
C5 C4 Os 71.6(5) . . ?
C3 C4 Os 69.5(5) . . ?
C8 C4 Os 128.7(6) . . ?
C6 C5 C4 121.6(9) . . ?
C6 C5 Os 71.5(5) . . ?
C4 C5 Os 70.7(5) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
Os C5 H5 131.6 . . ?
C5 C6 C1 120.3(10) . . ?
C5 C6 Os 71.2(5) . . ?
C1 C6 Os 70.3(6) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
Os C6 H6 131.5 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 C9 108.6(8) . . ?
C4 C8 C10 114.3(8) . . ?
C9 C8 C10 112.0(9) . . ?
C4 C8 H8 107.2 . . ?
C9 C8 H8 107.2 . . ?
C10 C8 H8 107.2 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 123.2(9) . . ?
N1 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C11 C12 C13 117.7(9) . . ?
C11 C12 H12 121.2 . . ?
C13 C12 H12 121.2 . . ?
C14 C13 C12 119.8(10) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C15 C14 C13 119.0(10) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
N1 C15 C14 122.2(9) . . ?
N1 C15 C16 116.6(8) . . ?
C14 C15 C16 121.1(9) . . ?
N2 C16 C15 107.2(8) . . ?
N2 C16 H16A 110.3 . . ?
C15 C16 H16A 110.3 . . ?
N2 C16 H16B 110.3 . . ?
C15 C16 H16B 110.3 . . ?
H16A C16 H16B 108.5 . . ?
N2 C17 N3 118.4(8) . . ?
N2 C17 N4 120.9(9) . . ?
N3 C17 N4 120.6(8) . . ?
C19 C18 C23 118.7(9) . . ?
C19 C18 N3 118.3(9) . . ?
C23 C18 N3 123.0(9) . . ?
C20 C19 C18 120.8(10) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 121.4(10) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C22 C21 C20 116.0(10) . . ?
C22 C21 C24 124.1(11) . . ?
C20 C21 C24 119.9(10) . . ?
C21 C22 C23 123.9(10) . . ?
C21 C22 H22 118.1 . . ?
C23 C22 H22 118.1 . . ?
C22 C23 C18 119.2(9) . . ?
C22 C23 H23 120.4 . . ?
C18 C23 H23 120.4 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 119.2(9) . . ?
C30 C25 N4 118.4(9) . . ?
C26 C25 N4 122.3(9) . . ?
C27 C26 C25 119.3(9) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C26 C27 C28 122.0(10) . . ?
C26 C27 H27 119.0 . . ?
C28 C27 H27 119.0 . . ?
C29 C28 C27 117.7(9) . . ?
C29 C28 C31 120.5(10) . . ?
C27 C28 C31 121.8(10) . . ?
C28 C29 C30 120.9(10) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C25 C30 C29 120.8(10) . . ?
C25 C30 H30 119.6 . . ?
C29 C30 H30 119.6 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
F3 Sb1 F4 179.0(3) . . ?
F3 Sb1 F6 90.4(3) . . ?
F4 Sb1 F6 89.2(3) . . ?
F3 Sb1 F5 89.9(3) . . ?
F4 Sb1 F5 90.4(3) . . ?
F6 Sb1 F5 178.5(3) . . ?
F3 Sb1 F1 89.9(3) . . ?
F4 Sb1 F1 91.0(3) . . ?
F6 Sb1 F1 90.8(3) . . ?
F5 Sb1 F1 90.7(3) . . ?
F3 Sb1 F2 89.2(3) . . ?
F4 Sb1 F2 89.9(3) . . ?
F6 Sb1 F2 90.1(2) . . ?
F5 Sb1 F2 88.5(2) . . ?
F1 Sb1 F2 178.8(3) . . ?
F9B Sb2 F12B 112.4(15) . . ?
F9B Sb2 F10B 169.0(12) . . ?
F12B Sb2 F10B 69.2(12) . . ?
F9B Sb2 F8 92.0(9) . . ?
F12B Sb2 F8 92.8(6) . . ?
F10A Sb2 F8 82.0(5) . . ?
F10B Sb2 F8 98.8(8) . . ?
F9B Sb2 F7 86.0(9) . . ?
F12B Sb2 F7 87.8(6) . . ?
F10A Sb2 F7 99.9(5) . . ?
F10B Sb2 F7 83.2(8) . . ?
F8 Sb2 F7 178.1(4) . . ?
F9B Sb2 F11B 87.8(11) . . ?
F12B Sb2 F11B 157.0(11) . . ?
F10B Sb2 F11B 88.8(9) . . ?
F8 Sb2 F11B 97.7(7) . . ?
F7 Sb2 F11B 82.4(7) . . ?
F10A Sb2 F12A 104.7(7) . . ?
F8 Sb2 F12A 87.5(5) . . ?
F7 Sb2 F12A 92.5(5) . . ?
F10A Sb2 F11A 88.8(6) . . ?
F8 Sb2 F11A 84.2(6) . . ?
F7 Sb2 F11A 95.3(6) . . ?
F12A Sb2 F11A 163.1(9) . . ?
F10A Sb2 F9A 170.9(6) . . ?
F8 Sb2 F9A 89.5(5) . . ?
F7 Sb2 F9A 88.6(5) . . ?
F12A Sb2 F9A 78.0(8) . . ?
F11A Sb2 F9A 87.2(6) . . ?
Cl1 C51 Cl2 112.5(6) . . ?
Cl1 C51 H51A 109.1 . . ?
Cl2 C51 H51A 109.1 . . ?
Cl1 C51 H51B 109.1 . . ?
Cl2 C51 H51B 109.1 . . ?
H51A C51 H51B 107.8 . . ?
Cl4 C52 Cl3 112.3(7) . . ?
Cl4 C52 H52A 109.1 . . ?
Cl3 C52 H52A 109.1 . . ?
Cl4 C52 H52B 109.1 . . ?
Cl3 C52 H52B 109.1 . . ?
H52A C52 H52B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -4.8(13) . . . . ?
C7 C1 C2 C3 176.5(9) . . . . ?
Os C1 C2 C3 51.4(8) . . . . ?
C6 C1 C2 Os -56.2(8) . . . . ?
C7 C1 C2 Os 125.1(9) . . . . ?
C1 C2 C3 C4 2.8(13) . . . . ?
Os C2 C3 C4 55.1(7) . . . . ?
C1 C2 C3 Os -52.2(8) . . . . ?
C2 C3 C4 C5 0.8(12) . . . . ?
Os C3 C4 C5 55.6(7) . . . . ?
C2 C3 C4 C8 -178.4(8) . . . . ?
Os C3 C4 C8 -123.6(8) . . . . ?
C2 C3 C4 Os -54.8(7) . . . . ?
C3 C4 C5 C6 -2.2(13) . . . . ?
C8 C4 C5 C6 177.1(8) . . . . ?
Os C4 C5 C6 52.4(8) . . . . ?
C3 C4 C5 Os -54.6(7) . . . . ?
C8 C4 C5 Os 124.7(8) . . . . ?
C4 C5 C6 C1 0.2(14) . . . . ?
Os C5 C6 C1 52.2(8) . . . . ?
C4 C5 C6 Os -52.0(8) . . . . ?
C2 C1 C6 C5 3.3(13) . . . . ?
C7 C1 C6 C5 -177.9(9) . . . . ?
Os C1 C6 C5 -52.7(8) . . . . ?
C2 C1 C6 Os 56.0(8) . . . . ?
C7 C1 C6 Os -125.3(8) . . . . ?
C5 C4 C8 C9 76.0(11) . . . . ?
C3 C4 C8 C9 -104.8(10) . . . . ?
Os C4 C8 C9 166.1(7) . . . . ?
C5 C4 C8 C10 -158.2(9) . . . . ?
C3 C4 C8 C10 21.0(13) . . . . ?
Os C4 C8 C10 -68.1(12) . . . . ?
C15 N1 C11 C12 -1.5(14) . . . . ?
Os N1 C11 C12 177.5(7) . . . . ?
N1 C11 C12 C13 1.6(15) . . . . ?
C11 C12 C13 C14 -0.8(15) . . . . ?
C12 C13 C14 C15 0.0(15) . . . . ?
C11 N1 C15 C14 0.7(13) . . . . ?
Os N1 C15 C14 -178.4(7) . . . . ?
C11 N1 C15 C16 -179.5(8) . . . . ?
Os N1 C15 C16 1.4(11) . . . . ?
C13 C14 C15 N1 0.0(15) . . . . ?
C13 C14 C15 C16 -179.8(9) . . . . ?
C17 N2 C16 C15 155.0(8) . . . . ?
Os N2 C16 C15 -31.6(9) . . . . ?
N1 C15 C16 N2 19.6(11) . . . . ?
C14 C15 C16 N2 -160.6(8) . . . . ?
C16 N2 C17 N3 -162.8(8) . . . . ?
Os N2 C17 N3 24.7(12) . . . . ?
C16 N2 C17 N4 14.8(13) . . . . ?
Os N2 C17 N4 -157.8(6) . . . . ?
C18 N3 C17 N2 -142.0(9) . . . . ?
C18 N3 C17 N4 40.4(13) . . . . ?
C25 N4 C17 N2 -159.7(9) . . . . ?
C25 N4 C17 N3 17.8(14) . . . . ?
C17 N3 C18 C19 -165.8(9) . . . . ?
C17 N3 C18 C23 14.9(14) . . . . ?
C23 C18 C19 C20 0.6(14) . . . . ?
N3 C18 C19 C20 -178.7(9) . . . . ?
C18 C19 C20 C21 -2.5(15) . . . . ?
C19 C20 C21 C22 2.4(15) . . . . ?
C19 C20 C21 C24 -176.1(10) . . . . ?
C20 C21 C22 C23 -0.3(14) . . . . ?
C24 C21 C22 C23 178.1(10) . . . . ?
C21 C22 C23 C18 -1.5(14) . . . . ?
C19 C18 C23 C22 1.4(13) . . . . ?
N3 C18 C23 C22 -179.3(8) . . . . ?
C17 N4 C25 C30 -141.8(10) . . . . ?
C17 N4 C25 C26 38.8(14) . . . . ?
C30 C25 C26 C27 1.1(14) . . . . ?
N4 C25 C26 C27 -179.6(9) . . . . ?
C25 C26 C27 C28 -1.7(15) . . . . ?
C26 C27 C28 C29 1.3(15) . . . . ?
C26 C27 C28 C31 -178.5(10) . . . . ?
C27 C28 C29 C30 -0.3(15) . . . . ?
C31 C28 C29 C30 179.5(10) . . . . ?
C26 C25 C30 C29 -0.1(15) . . . . ?
N4 C25 C30 C29 -179.5(9) . . . . ?
C28 C29 C30 C25 -0.3(16) . . . . ?

_refine_diff_density_max         2.354
_refine_diff_density_min         -2.100
_refine_diff_density_rms         0.233

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/hexane'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cmpnd_2
_database_code_depnum_ccdc_archive 'CCDC 1983331'
loop_
_audit_author_name
_audit_author_address
'Pilar Garcia-Orduna'
;Instituto de Sintesis Quimica y Catalisis Homogenea (ISQCH, CSIC Univ Zaragoza)
Spain
;
_audit_update_record             
;
2020-07-31 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H44 Cl N3 Os P, F6 Sb'
_chemical_formula_sum            'C39 H44 Cl F6 N3 Os P Sb'
_chemical_formula_weight         1047.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.9424(4)
_cell_length_b                   13.4216(5)
_cell_length_c                   25.9506(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3811.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9926
_cell_measurement_theta_min      2.435
_cell_measurement_theta_max      29.393

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_F_000             2048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.146
_exptl_absorpt_coefficient_mu    4.214
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3736
_exptl_absorpt_correction_T_max  0.5016
_exptl_absorpt_process_details   
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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 APEX DUO CCD system'
_diffrn_measurement_method       'narrow ω frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_decay_%        0
_diffrn_reflns_number            95284
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.569
_diffrn_reflns_theta_max         29.777
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10435
_reflns_number_gt                10312
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_max     0.940
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_cell_refinement       'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'

_refine_special_details          
;
Hydrogen atoms have been observed in Fourier difference maps. Those
of methyl and aromatic groups have been included in the model
in calculated positions and refined with a riding model.
Hydrogen atoms bounded to N2 and N3 atoms have been located
as observed positions. A geometrical restraint in N2-H2N bond length
has been used in the refinement. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0196P)²+2.7668P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Direct method'
_atom_sites_solution_secondary   'Fourier Difference Synthesis'
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 4470 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0031(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10435
_refine_ls_number_parameters     498
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0411
_refine_ls_wR_factor_gt          0.0409
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.38062(2) 0.63083(2) 0.74650(2) 0.01114(3) Uani 1 1 d . . . . .
P P 0.29150(7) 0.53842(6) 0.68049(3) 0.01324(15) Uani 1 1 d . . . . .
Cl Cl 0.52149(7) 0.49363(5) 0.74766(4) 0.01681(13) Uani 1 1 d . . . . .
N1 N 0.2741(3) 0.5312(2) 0.79241(10) 0.0149(5) Uani 1 1 d . . . . .
N2 N 0.4051(2) 0.5354(2) 0.86282(10) 0.0160(5) Uani 1 1 d D . . . .
N3 N 0.2119(3) 0.4642(2) 0.87164(11) 0.0179(6) Uani 1 1 d . . . . .
C1 C 0.5321(3) 0.7335(2) 0.72758(14) 0.0162(6) Uani 1 1 d . . . . .
C2 C 0.4266(3) 0.7633(2) 0.70036(13) 0.0158(6) Uani 1 1 d . . . . .
H2 H 0.4303 0.7707 0.6640 0.019 Uiso 1 1 calc R U . . .
C3 C 0.3141(3) 0.7825(2) 0.72662(13) 0.0163(6) Uani 1 1 d . . . . .
H3 H 0.2441 0.8021 0.7075 0.020 Uiso 1 1 calc R U . . .
C4 C 0.3059(3) 0.7725(2) 0.78058(13) 0.0152(6) Uani 1 1 d . . . . .
C5 C 0.4144(3) 0.7462(2) 0.80821(13) 0.0159(6) Uani 1 1 d . . . . .
H5 H 0.4117 0.7419 0.8447 0.019 Uiso 1 1 calc R U . . .
C6 C 0.5238(3) 0.7268(3) 0.78275(13) 0.0171(6) Uani 1 1 d . . . . .
H6 H 0.5941 0.7089 0.8021 0.021 Uiso 1 1 calc R U . . .
C7 C 0.6520(3) 0.7105(3) 0.70185(14) 0.0207(7) Uani 1 1 d . . . . .
H7A H 0.6374 0.6921 0.6658 0.031 Uiso 1 1 calc R U . . .
H7B H 0.6919 0.6551 0.7198 0.031 Uiso 1 1 calc R U . . .
H7C H 0.7048 0.7694 0.7032 0.031 Uiso 1 1 calc R U . . .
C8 C 0.1948(3) 0.8005(3) 0.81274(14) 0.0192(7) Uani 1 1 d . . . . .
H8 H 0.1931 0.7559 0.8436 0.023 Uiso 1 1 calc R U . . .
C9 C 0.2159(4) 0.9077(3) 0.83171(17) 0.0310(9) Uani 1 1 d . . . . .
H9A H 0.2931 0.9109 0.8508 0.047 Uiso 1 1 calc R U . . .
H9B H 0.1485 0.9275 0.8544 0.047 Uiso 1 1 calc R U . . .
H9C H 0.2196 0.9528 0.8021 0.047 Uiso 1 1 calc R U . . .
C10 C 0.0726(4) 0.7916(3) 0.78576(15) 0.0276(8) Uani 1 1 d . . . . .
H10A H 0.0726 0.8335 0.7548 0.041 Uiso 1 1 calc R U . . .
H10B H 0.0075 0.8135 0.8091 0.041 Uiso 1 1 calc R U . . .
H10C H 0.0586 0.7220 0.7759 0.041 Uiso 1 1 calc R U . . .
C11 C 0.2268(3) 0.4330(3) 0.71570(13) 0.0176(6) Uani 1 1 d . . . . .
C12 C 0.1765(3) 0.4742(3) 0.76622(13) 0.0170(6) Uani 1 1 d . . . . .
C13 C 0.3900(3) 0.4859(2) 0.63135(12) 0.0159(6) Uani 1 1 d . . . . .
C14 C 0.4800(3) 0.5449(3) 0.60847(14) 0.0219(7) Uani 1 1 d . . . . .
H14 H 0.4916 0.6114 0.6201 0.026 Uiso 1 1 calc R U . . .
C15 C 0.5529(4) 0.5081(3) 0.56887(15) 0.0264(8) Uani 1 1 d . . . . .
H15 H 0.6143 0.5489 0.5539 0.032 Uiso 1 1 calc R U . . .
C16 C 0.5355(4) 0.4114(3) 0.55140(15) 0.0265(8) Uani 1 1 d . . . . .
H16 H 0.5837 0.3862 0.5239 0.032 Uiso 1 1 calc R U . . .
C17 C 0.4475(4) 0.3516(3) 0.57420(15) 0.0258(8) Uani 1 1 d . . . . .
H17 H 0.4369 0.2850 0.5626 0.031 Uiso 1 1 calc R U . . .
C18 C 0.3746(3) 0.3880(2) 0.61394(13) 0.0208(6) Uani 1 1 d . . . . .
H18 H 0.3143 0.3464 0.6292 0.025 Uiso 1 1 calc R U . . .
C19 C 0.1608(3) 0.5859(2) 0.64427(13) 0.0160(6) Uani 1 1 d . . . . .
C20 C 0.0779(3) 0.6467(3) 0.66963(14) 0.0230(7) Uani 1 1 d . . . . .
H20 H 0.0942 0.6676 0.7039 0.028 Uiso 1 1 calc R U . . .
C21 C -0.0289(4) 0.6772(3) 0.64534(17) 0.0290(8) Uani 1 1 d . . . . .
H21 H -0.0858 0.7180 0.6632 0.035 Uiso 1 1 calc R U . . .
C22 C -0.0525(4) 0.6483(3) 0.59509(16) 0.0285(8) Uani 1 1 d . . . . .
H22 H -0.1254 0.6693 0.5784 0.034 Uiso 1 1 calc R U . . .
C23 C 0.0305(4) 0.5888(3) 0.56936(15) 0.0259(8) Uani 1 1 d . . . . .
H23 H 0.0144 0.5693 0.5348 0.031 Uiso 1 1 calc R U . . .
C24 C 0.1372(4) 0.5570(2) 0.59336(13) 0.0214(7) Uani 1 1 d . . . . .
H24 H 0.1938 0.5161 0.5754 0.026 Uiso 1 1 calc R U . . .
C25 C 0.2958(3) 0.5110(2) 0.84118(13) 0.0160(6) Uani 1 1 d . . . . .
C26 C 0.4210(3) 0.5742(2) 0.91320(12) 0.0160(6) Uani 1 1 d . . . . .
C27 C 0.5345(3) 0.5633(3) 0.93701(13) 0.0198(7) Uani 1 1 d . . . . .
H27 H 0.5983 0.5278 0.9202 0.024 Uiso 1 1 calc R U . . .
C28 C 0.5537(4) 0.6047(3) 0.98548(14) 0.0249(8) Uani 1 1 d . . . . .
H28 H 0.6314 0.5976 1.0014 0.030 Uiso 1 1 calc R U . . .
C29 C 0.4619(4) 0.6560(3) 1.01111(14) 0.0259(8) Uani 1 1 d . . . . .
C30 C 0.3492(4) 0.6653(3) 0.98709(14) 0.0246(8) Uani 1 1 d . . . . .
H30 H 0.2848 0.6991 1.0043 0.029 Uiso 1 1 calc R U . . .
C31 C 0.3287(3) 0.6259(3) 0.93813(13) 0.0209(7) Uani 1 1 d . . . . .
H31 H 0.2516 0.6344 0.9219 0.025 Uiso 1 1 calc R U . . .
C32 C 0.4849(5) 0.7016(4) 1.06365(17) 0.0406(11) Uani 1 1 d . . . . .
H32A H 0.5160 0.7696 1.0594 0.061 Uiso 1 1 calc R U . . .
H32B H 0.5452 0.6614 1.0823 0.061 Uiso 1 1 calc R U . . .
H32C H 0.4083 0.7034 1.0832 0.061 Uiso 1 1 calc R U . . .
C33 C 0.2351(3) 0.4034(2) 0.91509(13) 0.0159(6) Uani 1 1 d . . . . .
C34 C 0.3380(3) 0.3436(2) 0.91873(14) 0.0198(7) Uani 1 1 d . . . . .
H34 H 0.3990 0.3459 0.8927 0.024 Uiso 1 1 calc R U . . .
C35 C 0.3514(4) 0.2802(3) 0.96078(15) 0.0240(7) Uani 1 1 d . . . . .
H35 H 0.4223 0.2396 0.9629 0.029 Uiso 1 1 calc R U . . .
C36 C 0.2651(4) 0.2742(3) 0.99970(14) 0.0232(7) Uani 1 1 d . . . . .
C37 C 0.1648(4) 0.3369(3) 0.99596(14) 0.0234(8) Uani 1 1 d . . . . .
H37 H 0.1053 0.3362 1.0226 0.028 Uiso 1 1 calc R U . . .
C38 C 0.1487(3) 0.4011(3) 0.95426(13) 0.0204(7) Uani 1 1 d . . . . .
H38 H 0.0790 0.4431 0.9527 0.024 Uiso 1 1 calc R U . . .
C39 C 0.2782(5) 0.2030(3) 1.04441(16) 0.0355(10) Uani 1 1 d . . . . .
H39A H 0.2515 0.2359 1.0762 0.053 Uiso 1 1 calc R U . . .
H39B H 0.3640 0.1831 1.0478 0.053 Uiso 1 1 calc R U . . .
H39C H 0.2277 0.1439 1.0382 0.053 Uiso 1 1 calc R U . . .
Sb Sb 0.85577(2) 0.54546(2) 0.85163(2) 0.02066(5) Uani 1 1 d . . . . .
F1 F 1.00887(19) 0.60930(16) 0.85722(10) 0.0280(5) Uani 1 1 d . . . . .
F2 F 0.7085(2) 0.4753(2) 0.84750(10) 0.0383(6) Uani 1 1 d . . . . .
F3 F 0.7741(2) 0.66800(19) 0.85260(11) 0.0382(6) Uani 1 1 d . . . . .
F4 F 0.9417(2) 0.42396(17) 0.85013(10) 0.0304(5) Uani 1 1 d . . . . .
F5 F 0.8670(3) 0.5532(2) 0.77997(9) 0.0389(6) Uani 1 1 d . . . . .
F6 F 0.8480(2) 0.53993(19) 0.92367(8) 0.0300(5) Uani 1 1 d . . . . .
H11A H 0.170(4) 0.401(3) 0.7007(15) 0.016(10) Uiso 1 1 d . . . . .
H11B H 0.295(4) 0.389(3) 0.7208(16) 0.020(11) Uiso 1 1 d . . . . .
H12A H 0.107(3) 0.518(3) 0.7613(14) 0.013(9) Uiso 1 1 d . . . . .
H12B H 0.149(4) 0.418(3) 0.7874(16) 0.022(11) Uiso 1 1 d . . . . .
H2N H 0.466(3) 0.533(3) 0.8431(15) 0.024(11) Uiso 1 1 d D . . . .
H3N H 0.138(4) 0.472(3) 0.8637(15) 0.013(9) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os N1 2.136(3) . ?
Os C2 2.201(3) . ?
Os C1 2.211(3) . ?
Os C3 2.222(3) . ?
Os C6 2.236(3) . ?
Os C4 2.251(3) . ?
Os C5 2.258(3) . ?
Os P 2.3289(8) . ?
Os Cl 2.4017(7) . ?
P C13 1.812(3) . ?
P C19 1.826(3) . ?
P C11 1.827(3) . ?
N1 C25 1.316(4) . ?
N1 C12 1.480(4) . ?
N2 C25 1.361(4) . ?
N2 C26 1.418(4) . ?
N2 H2N 0.84(2) . ?
N3 C25 1.365(4) . ?
N3 C33 1.415(4) . ?
N3 H3N 0.84(4) . ?
C1 C2 1.411(5) . ?
C1 C6 1.437(5) . ?
C1 C7 1.504(5) . ?
C2 C3 1.430(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.410(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.431(5) . ?
C4 C8 1.522(5) . ?
C5 C6 1.392(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.514(5) . ?
C8 C9 1.538(5) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.526(5) . ?
C11 H11A 0.85(4) . ?
C11 H11B 0.96(4) . ?
C12 H12A 0.97(4) . ?
C12 H12B 0.98(4) . ?
C13 C14 1.396(5) . ?
C13 C18 1.400(4) . ?
C14 C15 1.392(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.393(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.386(5) . ?
C19 C24 1.401(5) . ?
C20 C21 1.390(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.385(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.390(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C26 C31 1.385(5) . ?
C26 C27 1.395(5) . ?
C27 C28 1.391(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.388(6) . ?
C29 C32 1.516(5) . ?
C30 C31 1.394(5) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.386(5) . ?
C33 C38 1.388(5) . ?
C34 C35 1.391(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.385(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.386(6) . ?
C36 C39 1.510(5) . ?
C37 C38 1.394(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
Sb F5 1.867(2) . ?
Sb F2 1.869(2) . ?
Sb F3 1.872(2) . ?
Sb F6 1.873(2) . ?
Sb F4 1.883(2) . ?
Sb F1 1.887(2) . ?

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 Os C2 158.93(12) . . ?
N1 Os C1 157.34(12) . . ?
C2 Os C1 37.31(13) . . ?
N1 Os C3 121.59(12) . . ?
C2 Os C3 37.73(13) . . ?
C1 Os C3 67.87(13) . . ?
N1 Os C6 120.53(11) . . ?
C2 Os C6 66.65(13) . . ?
C1 Os C6 37.71(12) . . ?
C3 Os C6 78.44(13) . . ?
N1 Os C4 96.40(12) . . ?
C2 Os C4 67.32(12) . . ?
C1 Os C4 80.38(13) . . ?
C3 Os C4 36.73(11) . . ?
C6 Os C4 66.57(13) . . ?
N1 Os C5 97.06(12) . . ?
C2 Os C5 78.14(12) . . ?
C1 Os C5 66.87(13) . . ?
C3 Os C5 65.81(12) . . ?
C6 Os C5 36.08(13) . . ?
C4 Os C5 37.01(12) . . ?
N1 Os P 81.29(8) . . ?
C2 Os P 97.22(9) . . ?
C1 Os P 118.85(9) . . ?
C3 Os P 100.36(9) . . ?
C6 Os P 155.47(9) . . ?
C4 Os P 125.94(9) . . ?
C5 Os P 162.83(9) . . ?
N1 Os Cl 82.15(8) . . ?
C2 Os Cl 118.64(9) . . ?
C1 Os Cl 89.97(9) . . ?
C3 Os Cl 156.26(9) . . ?
C6 Os Cl 89.23(9) . . ?
C4 Os Cl 151.15(9) . . ?
C5 Os Cl 114.32(9) . . ?
P Os Cl 82.51(3) . . ?
C13 P C19 103.85(15) . . ?
C13 P C11 106.34(16) . . ?
C19 P C11 102.97(16) . . ?
C13 P Os 118.38(11) . . ?
C19 P Os 121.37(11) . . ?
C11 P Os 101.94(11) . . ?
C25 N1 C12 117.7(3) . . ?
C25 N1 Os 124.5(2) . . ?
C12 N1 Os 117.5(2) . . ?
C25 N2 C26 125.2(3) . . ?
C25 N2 H2N 116(3) . . ?
C26 N2 H2N 119(3) . . ?
C25 N3 C33 127.3(3) . . ?
C25 N3 H3N 117(3) . . ?
C33 N3 H3N 116(3) . . ?
C2 C1 C6 117.7(3) . . ?
C2 C1 C7 123.3(3) . . ?
C6 C1 C7 119.0(3) . . ?
C2 C1 Os 70.97(19) . . ?
C6 C1 Os 72.1(2) . . ?
C7 C1 Os 128.7(2) . . ?
C1 C2 C3 121.1(3) . . ?
C1 C2 Os 71.72(19) . . ?
C3 C2 Os 71.93(19) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
Os C2 H2 129.4 . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 Os 72.7(2) . . ?
C2 C3 Os 70.34(19) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
Os C3 H3 129.8 . . ?
C3 C4 C5 117.9(3) . . ?
C3 C4 C8 124.9(3) . . ?
C5 C4 C8 116.7(3) . . ?
C3 C4 Os 70.5(2) . . ?
C5 C4 Os 71.78(19) . . ?
C8 C4 Os 135.5(2) . . ?
C6 C5 C4 121.5(3) . . ?
C6 C5 Os 71.09(19) . . ?
C4 C5 Os 71.22(19) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
Os C5 H5 131.3 . . ?
C5 C6 C1 121.0(3) . . ?
C5 C6 Os 72.8(2) . . ?
C1 C6 Os 70.2(2) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
Os C6 H6 130.1 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C4 115.6(3) . . ?
C10 C8 C9 110.8(3) . . ?
C4 C8 C9 106.6(3) . . ?
C10 C8 H8 107.9 . . ?
C4 C8 H8 107.9 . . ?
C9 C8 H8 107.9 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 P 106.8(2) . . ?
C12 C11 H11A 108(3) . . ?
P C11 H11A 116(3) . . ?
C12 C11 H11B 113(3) . . ?
P C11 H11B 104(3) . . ?
H11A C11 H11B 109(4) . . ?
N1 C12 C11 108.7(3) . . ?
N1 C12 H12A 108(2) . . ?
C11 C12 H12A 113(2) . . ?
N1 C12 H12B 111(3) . . ?
C11 C12 H12B 108(2) . . ?
H12A C12 H12B 108(3) . . ?
C14 C13 C18 118.7(3) . . ?
C14 C13 P 119.9(2) . . ?
C18 C13 P 121.3(3) . . ?
C15 C14 C13 121.1(3) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C16 C15 C14 119.6(4) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C17 C16 C15 119.8(4) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 120.7(3) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C13 119.9(3) . . ?
C17 C18 H18 120.0 . . ?
C13 C18 H18 120.0 . . ?
C20 C19 C24 119.3(3) . . ?
C20 C19 P 118.3(3) . . ?
C24 C19 P 122.2(3) . . ?
C19 C20 C21 120.6(3) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C22 C21 C20 120.1(4) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C23 C22 C21 119.6(4) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C24 120.9(4) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C19 119.5(3) . . ?
C23 C24 H24 120.3 . . ?
C19 C24 H24 120.3 . . ?
N1 C25 N2 120.4(3) . . ?
N1 C25 N3 122.0(3) . . ?
N2 C25 N3 117.6(3) . . ?
C31 C26 C27 119.7(3) . . ?
C31 C26 N2 121.7(3) . . ?
C27 C26 N2 118.6(3) . . ?
C28 C27 C26 119.5(3) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C29 C28 C27 121.5(4) . . ?
C29 C28 H28 119.2 . . ?
C27 C28 H28 119.2 . . ?
C28 C29 C30 118.2(3) . . ?
C28 C29 C32 120.8(4) . . ?
C30 C29 C32 121.0(4) . . ?
C29 C30 C31 121.2(4) . . ?
C29 C30 H30 119.4 . . ?
C31 C30 H30 119.4 . . ?
C26 C31 C30 119.9(3) . . ?
C26 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C38 119.4(3) . . ?
C34 C33 N3 122.3(3) . . ?
C38 C33 N3 118.3(3) . . ?
C33 C34 C35 119.5(3) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C36 C35 C34 122.4(3) . . ?
C36 C35 H35 118.8 . . ?
C34 C35 H35 118.8 . . ?
C35 C36 C37 117.0(3) . . ?
C35 C36 C39 122.1(4) . . ?
C37 C36 C39 120.9(4) . . ?
C36 C37 C38 122.0(3) . . ?
C36 C37 H37 119.0 . . ?
C38 C37 H37 119.0 . . ?
C33 C38 C37 119.7(3) . . ?
C33 C38 H38 120.1 . . ?
C37 C38 H38 120.1 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
F5 Sb F2 91.60(12) . . ?
F5 Sb F3 89.77(12) . . ?
F2 Sb F3 91.80(13) . . ?
F5 Sb F6 178.50(12) . . ?
F2 Sb F6 89.89(11) . . ?
F3 Sb F6 89.98(12) . . ?
F5 Sb F4 89.69(11) . . ?
F2 Sb F4 89.60(12) . . ?
F3 Sb F4 178.52(12) . . ?
F6 Sb F4 90.52(11) . . ?
F5 Sb F1 89.58(12) . . ?
F2 Sb F1 176.61(12) . . ?
F3 Sb F1 91.38(12) . . ?
F6 Sb F1 88.94(11) . . ?
F4 Sb F1 87.23(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -2.3(5) . . . . ?
C7 C1 C2 C3 178.8(3) . . . . ?
Os C1 C2 C3 54.5(3) . . . . ?
C6 C1 C2 Os -56.8(3) . . . . ?
C7 C1 C2 Os 124.3(3) . . . . ?
C1 C2 C3 C4 0.3(5) . . . . ?
Os C2 C3 C4 54.7(3) . . . . ?
C1 C2 C3 Os -54.4(3) . . . . ?
C2 C3 C4 C5 2.2(5) . . . . ?
Os C3 C4 C5 55.7(3) . . . . ?
C2 C3 C4 C8 173.9(3) . . . . ?
Os C3 C4 C8 -132.6(3) . . . . ?
C2 C3 C4 Os -53.5(3) . . . . ?
C3 C4 C5 C6 -2.6(5) . . . . ?
C8 C4 C5 C6 -175.0(3) . . . . ?
Os C4 C5 C6 52.5(3) . . . . ?
C3 C4 C5 Os -55.1(3) . . . . ?
C8 C4 C5 Os 132.5(3) . . . . ?
C4 C5 C6 C1 0.6(5) . . . . ?
Os C5 C6 C1 53.1(3) . . . . ?
C4 C5 C6 Os -52.5(3) . . . . ?
C2 C1 C6 C5 1.8(5) . . . . ?
C7 C1 C6 C5 -179.2(3) . . . . ?
Os C1 C6 C5 -54.4(3) . . . . ?
C2 C1 C6 Os 56.2(3) . . . . ?
C7 C1 C6 Os -124.9(3) . . . . ?
C3 C4 C8 C10 29.5(5) . . . . ?
C5 C4 C8 C10 -158.7(3) . . . . ?
Os C4 C8 C10 -68.0(5) . . . . ?
C3 C4 C8 C9 -94.1(4) . . . . ?
C5 C4 C8 C9 77.7(4) . . . . ?
Os C4 C8 C9 168.4(3) . . . . ?
C13 P C11 C12 163.1(2) . . . . ?
C19 P C11 C12 -88.0(2) . . . . ?
Os P C11 C12 38.5(2) . . . . ?
C25 N1 C12 C11 -129.8(3) . . . . ?
Os N1 C12 C11 44.6(3) . . . . ?
P C11 C12 N1 -53.1(3) . . . . ?
C19 P C13 C14 91.1(3) . . . . ?
C11 P C13 C14 -160.7(3) . . . . ?
Os P C13 C14 -46.9(3) . . . . ?
C19 P C13 C18 -86.0(3) . . . . ?
C11 P C13 C18 22.2(3) . . . . ?
Os P C13 C18 136.0(2) . . . . ?
C18 C13 C14 C15 0.4(5) . . . . ?
P C13 C14 C15 -176.8(3) . . . . ?
C13 C14 C15 C16 0.6(6) . . . . ?
C14 C15 C16 C17 -1.4(6) . . . . ?
C15 C16 C17 C18 1.2(6) . . . . ?
C16 C17 C18 C13 -0.2(6) . . . . ?
C14 C13 C18 C17 -0.6(5) . . . . ?
P C13 C18 C17 176.6(3) . . . . ?
C13 P C19 C20 -168.8(3) . . . . ?
C11 P C19 C20 80.5(3) . . . . ?
Os P C19 C20 -32.4(3) . . . . ?
C13 P C19 C24 16.1(3) . . . . ?
C11 P C19 C24 -94.6(3) . . . . ?
Os P C19 C24 152.5(2) . . . . ?
C24 C19 C20 C21 1.3(5) . . . . ?
P C19 C20 C21 -174.0(3) . . . . ?
C19 C20 C21 C22 -1.0(6) . . . . ?
C20 C21 C22 C23 0.2(6) . . . . ?
C21 C22 C23 C24 0.3(6) . . . . ?
C22 C23 C24 C19 0.0(6) . . . . ?
C20 C19 C24 C23 -0.8(5) . . . . ?
P C19 C24 C23 174.3(3) . . . . ?
C12 N1 C25 N2 159.0(3) . . . . ?
Os N1 C25 N2 -15.0(4) . . . . ?
C12 N1 C25 N3 -20.0(5) . . . . ?
Os N1 C25 N3 165.9(2) . . . . ?
C26 N2 C25 N1 140.2(3) . . . . ?
C26 N2 C25 N3 -40.7(5) . . . . ?
C33 N3 C25 N1 152.2(3) . . . . ?
C33 N3 C25 N2 -26.9(5) . . . . ?
C25 N2 C26 C31 -25.0(5) . . . . ?
C25 N2 C26 C27 157.7(3) . . . . ?
C31 C26 C27 C28 -0.2(5) . . . . ?
N2 C26 C27 C28 177.2(3) . . . . ?
C26 C27 C28 C29 0.7(5) . . . . ?
C27 C28 C29 C30 0.0(5) . . . . ?
C27 C28 C29 C32 -179.3(4) . . . . ?
C28 C29 C30 C31 -1.1(5) . . . . ?
C32 C29 C30 C31 178.1(4) . . . . ?
C27 C26 C31 C30 -0.9(5) . . . . ?
N2 C26 C31 C30 -178.2(3) . . . . ?
C29 C30 C31 C26 1.6(5) . . . . ?
C25 N3 C33 C34 -32.9(5) . . . . ?
C25 N3 C33 C38 149.7(4) . . . . ?
C38 C33 C34 C35 1.9(5) . . . . ?
N3 C33 C34 C35 -175.5(3) . . . . ?
C33 C34 C35 C36 0.0(6) . . . . ?
C34 C35 C36 C37 -1.9(6) . . . . ?
C34 C35 C36 C39 178.1(4) . . . . ?
C35 C36 C37 C38 2.0(5) . . . . ?
C39 C36 C37 C38 -178.0(4) . . . . ?
C34 C33 C38 C37 -1.8(5) . . . . ?
N3 C33 C38 C37 175.7(3) . . . . ?
C36 C37 C38 C33 -0.2(6) . . . . ?

_refine_diff_density_max         1.255
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.086

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane/hexane'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cmpnd_8
_database_code_depnum_ccdc_archive 'CCDC 1983335'
loop_
_audit_author_name
_audit_author_address
'Pilar Garcia-Orduna'
;Instituto de Sintesis Quimica y Catalisis Homogenea (ISQCH, CSIC Univ Zaragoza)
Spain
;
_audit_update_record             
;
2020-07-31 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H36 N4 O Os, 2(F6 Sb),1.75(C H2 Cl2)'
_chemical_formula_sum            'C33.75 H39.50 Cl3.50 F12 N4 O Os Sb2'
_chemical_formula_weight         1302.97

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   16.9772(9)
_cell_length_b                   17.1277(9)
_cell_length_c                   17.5280(9)
_cell_angle_alpha                84.7380(10)
_cell_angle_beta                 66.4340(10)
_cell_angle_gamma                67.5710(10)
_cell_volume                     4307.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      2.369
_cell_measurement_theta_max      27.916

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_F_000             2494
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.115
_exptl_absorpt_coefficient_mu    4.491
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4426
_exptl_absorpt_correction_T_max  0.5750
_exptl_absorpt_process_details   
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(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 APEX CCD system'
_diffrn_measurement_method       'narrow ω frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_decay_%        0
_diffrn_reflns_number            64380
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.289
_diffrn_reflns_theta_max         28.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             20155
_reflns_number_gt                14839
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_cell_refinement       'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'

_refine_special_details          
;
The sample is found to be quite fragile. Crystals were coated in protecting 
perfluoropolyether oil. However, some of them split into layers when handling
them. Several crystals were tested before selecting the one used in 
the data collection, checking the indexation (dismissing twin existence)
and trying to maximize diffracted intensity. 
After selection and testing the crystals, the remained non-used sample was 
inspected. Crystals were found to be cracked.

The asymmetric unit contains two half-sandwich osmium complex molecules,
four SbF6 counterions and 3.5 dichloromethane solvent.

Most of the hydrogen atoms have been included in the model in calculated
positions and refined with a riding model. Those of N-H fragments
have been included in observed positions.Isotropic thermal parameters 
of these hydrogen atoms have been constrained to be 1.2 times those
of the coordinated nitrogen. A geometrical restraint has been defined
for N4-H4N bond length. 

Geometrical restraints concerning C-Cl bond lengths have been included in
the refinement. 

At the end of the refinement, when convergence is achieved, several residual
density peaks higher than 1 e/A^3 are observed. They are close to heavy atoms
(Sb or Os) or solvent molecules. They have no chemical sense.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1156P)²+40.1291P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Direct method'
_atom_sites_solution_secondary   'Fourier Difference Synthesis'
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         20155
_refine_ls_number_parameters     1059
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0690
_refine_ls_wR_factor_ref         0.2048
_refine_ls_wR_factor_gt          0.1818
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.65392(3) 0.31178(2) 0.17609(2) 0.02851(11) Uani 1 1 d . . . . .
O1 O 0.7581(7) 0.1236(5) 0.1291(5) 0.053(2) Uani 1 1 d . . . . .
N1 N 0.5332(6) 0.2896(5) 0.2432(5) 0.0282(16) Uani 1 1 d . . . . .
N2 N 0.6499(6) 0.3025(5) 0.2977(5) 0.0318(18) Uani 1 1 d . . . . .
N3 N 0.8076(7) 0.2581(6) 0.2641(6) 0.042(2) Uani 1 1 d . . . . .
H3N H 0.832(9) 0.227(8) 0.220(8) 0.050 Uiso 1 1 d . U . . .
N4 N 0.7020(7) 0.3037(5) 0.4016(6) 0.0366(19) Uani 1 1 d D . . . .
H4N H 0.643(2) 0.333(6) 0.427(7) 0.044 Uiso 1 1 d D U . . .
C1 C 0.7651(7) 0.3448(6) 0.0684(6) 0.034(2) Uani 1 1 d . . . . .
C2 C 0.7008(8) 0.3369(6) 0.0412(6) 0.035(2) Uani 1 1 d . . . . .
H2 H 0.7232 0.2991 -0.0058 0.042 Uiso 1 1 calc R U . . .
C3 C 0.6054(7) 0.3824(6) 0.0805(5) 0.031(2) Uani 1 1 d . . . . .
H3 H 0.5641 0.3718 0.0627 0.037 Uiso 1 1 calc R U . . .
C4 C 0.5690(7) 0.4456(6) 0.1480(5) 0.030(2) Uani 1 1 d . . . . .
C5 C 0.6323(7) 0.4526(5) 0.1769(6) 0.030(2) Uani 1 1 d . . . . .
H5 H 0.6108 0.4931 0.2215 0.035 Uiso 1 1 calc R U . . .
C6 C 0.7293(7) 0.3995(6) 0.1401(6) 0.031(2) Uani 1 1 d . . . . .
H6 H 0.7697 0.4012 0.1642 0.037 Uiso 1 1 calc R U . . .
C7 C 0.8669(8) 0.2959(8) 0.0273(8) 0.049(3) Uani 1 1 d . . . . .
H7A H 0.8781 0.2392 0.0082 0.074 Uiso 1 1 calc R U . . .
H7B H 0.8953 0.2911 0.0673 0.074 Uiso 1 1 calc R U . . .
H7C H 0.8942 0.3252 -0.0206 0.074 Uiso 1 1 calc R U . . .
C8 C 0.4667(7) 0.4969(6) 0.1853(6) 0.035(2) Uani 1 1 d . . . . .
H8 H 0.4330 0.4583 0.1914 0.042 Uiso 1 1 calc R U . . .
C9 C 0.4429(8) 0.5630(8) 0.1262(7) 0.047(3) Uani 1 1 d . . . . .
H9A H 0.4696 0.6051 0.1245 0.071 Uiso 1 1 calc R U . . .
H9B H 0.3753 0.5911 0.1456 0.071 Uiso 1 1 calc R U . . .
H9C H 0.4684 0.5357 0.0701 0.071 Uiso 1 1 calc R U . . .
C10 C 0.4327(9) 0.5412(8) 0.2708(8) 0.055(3) Uani 1 1 d . . . . .
H10A H 0.4368 0.4989 0.3121 0.083 Uiso 1 1 calc R U . . .
H10B H 0.3680 0.5806 0.2872 0.083 Uiso 1 1 calc R U . . .
H10C H 0.4714 0.5726 0.2679 0.083 Uiso 1 1 calc R U . . .
C11 C 0.4837(8) 0.2703(6) 0.2075(6) 0.034(2) Uani 1 1 d . . . . .
H11 H 0.5062 0.2638 0.1484 0.041 Uiso 1 1 calc R U . . .
C12 C 0.4033(8) 0.2605(7) 0.2550(6) 0.040(2) Uani 1 1 d . . . . .
H12 H 0.3695 0.2482 0.2289 0.047 Uiso 1 1 calc R U . . .
C13 C 0.3695(8) 0.2680(7) 0.3410(6) 0.043(3) Uani 1 1 d . . . . .
H13 H 0.3127 0.2616 0.3743 0.051 Uiso 1 1 calc R U . . .
C14 C 0.4205(8) 0.2852(6) 0.3774(6) 0.038(2) Uani 1 1 d . . . . .
H14 H 0.4001 0.2889 0.4364 0.046 Uiso 1 1 calc R U . . .
C15 C 0.5000(8) 0.2967(6) 0.3282(6) 0.032(2) Uani 1 1 d . . . . .
C16 C 0.5582(7) 0.3187(6) 0.3618(6) 0.032(2) Uani 1 1 d . . . . .
H16A H 0.5280 0.3793 0.3820 0.038 Uiso 1 1 calc R U . . .
H16B H 0.5632 0.2846 0.4096 0.038 Uiso 1 1 calc R U . . .
C17 C 0.7188(8) 0.2876(6) 0.3205(7) 0.036(2) Uani 1 1 d . . . . .
C18 C 0.8752(9) 0.2894(9) 0.2596(7) 0.050(3) Uani 1 1 d . . . . .
C19 C 0.9642(11) 0.2426(11) 0.2200(8) 0.070(4) Uani 1 1 d . . . . .
H19 H 0.9834 0.1878 0.1954 0.085 Uiso 1 1 calc R U . . .
C20 C 1.0341(13) 0.2785(13) 0.2147(12) 0.092(6) Uani 1 1 d . . . . .
H20 H 1.0986 0.2461 0.1880 0.111 Uiso 1 1 calc R U . . .
C21 C 1.0044(11) 0.3555(13) 0.2475(9) 0.076(5) Uani 1 1 d . . . . .
C22 C 0.9160(11) 0.4023(11) 0.2878(9) 0.070(4) Uani 1 1 d . . . . .
H22 H 0.8978 0.4572 0.3117 0.084 Uiso 1 1 calc R U . . .
C23 C 0.8494(11) 0.3703(9) 0.2950(8) 0.062(4) Uani 1 1 d . . . . .
H23 H 0.7855 0.4037 0.3243 0.074 Uiso 1 1 calc R U . . .
C24 C 1.0815(15) 0.3897(17) 0.2323(11) 0.119(9) Uani 1 1 d . . . . .
H24A H 1.1015 0.4080 0.1754 0.179 Uiso 1 1 calc R U . . .
H24B H 1.1345 0.3448 0.2394 0.179 Uiso 1 1 calc R U . . .
H24C H 1.0573 0.4379 0.2724 0.179 Uiso 1 1 calc R U . . .
C25 C 0.7655(8) 0.2678(7) 0.4412(6) 0.038(2) Uani 1 1 d . . . . .
C26 C 0.8259(7) 0.1836(7) 0.4262(7) 0.040(2) Uani 1 1 d . . . . .
H26 H 0.8280 0.1477 0.3866 0.047 Uiso 1 1 calc R U . . .
C27 C 0.8824(8) 0.1526(8) 0.4690(7) 0.045(3) Uani 1 1 d . . . . .
H27 H 0.9236 0.0949 0.4581 0.054 Uiso 1 1 calc R U . . .
C28 C 0.8816(8) 0.2017(8) 0.5268(7) 0.044(3) Uani 1 1 d . . . . .
C29 C 0.8209(10) 0.2850(8) 0.5420(8) 0.052(3) Uani 1 1 d . . . . .
H29 H 0.8188 0.3198 0.5825 0.062 Uiso 1 1 calc R U . . .
C30 C 0.7620(9) 0.3200(7) 0.4994(7) 0.047(3) Uani 1 1 d . . . . .
H30 H 0.7209 0.3778 0.5102 0.057 Uiso 1 1 calc R U . . .
C31 C 0.9408(10) 0.1668(10) 0.5772(9) 0.063(4) Uani 1 1 d . . . . .
H31A H 0.9085 0.1418 0.6263 0.094 Uiso 1 1 calc R U . . .
H31B H 0.9519 0.2127 0.5952 0.094 Uiso 1 1 calc R U . . .
H31C H 1.0003 0.1233 0.5427 0.094 Uiso 1 1 calc R U . . .
C32 C 0.7181(8) 0.1939(6) 0.1490(6) 0.037(2) Uani 1 1 d . . . . .
Os51 Os 0.64679(3) 0.80735(2) 0.17345(2) 0.02787(11) Uani 1 1 d . . . . .
O51 O 0.7259(6) 0.6156(5) 0.1469(5) 0.049(2) Uani 1 1 d . . . . .
N51 N 0.5165(5) 0.8066(5) 0.2500(5) 0.0260(15) Uani 1 1 d . . . . .
N52 N 0.6467(6) 0.8038(5) 0.2935(4) 0.0280(16) Uani 1 1 d . . . . .
N53 N 0.8006(7) 0.7194(6) 0.2606(6) 0.038(2) Uani 1 1 d . . . . .
H53N H 0.794(8) 0.687(8) 0.237(7) 0.045 Uiso 1 1 d . U . . .
N54 N 0.7117(6) 0.8025(5) 0.3876(5) 0.0302(17) Uani 1 1 d . . . . .
H54N H 0.670(8) 0.859(7) 0.405(7) 0.036 Uiso 1 1 d . U . . .
C51 C 0.7676(9) 0.8229(9) 0.0626(7) 0.048(3) Uani 1 1 d . . . . .
C52 C 0.6998(8) 0.8203(7) 0.0361(6) 0.042(3) Uani 1 1 d . . . . .
H52 H 0.7187 0.7803 -0.0081 0.050 Uiso 1 1 calc R U . . .
C53 C 0.6066(8) 0.8741(6) 0.0721(6) 0.034(2) Uani 1 1 d . . . . .
H53 H 0.5632 0.8665 0.0553 0.041 Uiso 1 1 calc R U . . .
C54 C 0.5752(8) 0.9404(6) 0.1339(6) 0.038(2) Uani 1 1 d . . . . .
C55 C 0.6415(9) 0.9431(7) 0.1621(6) 0.042(3) Uani 1 1 d . . . . .
H55 H 0.6232 0.9862 0.2031 0.050 Uiso 1 1 calc R U . . .
C56 C 0.7355(8) 0.8827(7) 0.1308(7) 0.041(3) Uani 1 1 d . . . . .
H56 H 0.7763 0.8824 0.1554 0.049 Uiso 1 1 calc R U . . .
C57 C 0.8691(10) 0.7591(12) 0.0242(9) 0.077(5) Uani 1 1 d . . . . .
H57A H 0.8701 0.7037 0.0128 0.116 Uiso 1 1 calc R U . . .
H57B H 0.8985 0.7539 0.0635 0.116 Uiso 1 1 calc R U . . .
H57C H 0.9031 0.7792 -0.0280 0.116 Uiso 1 1 calc R U . . .
C58 C 0.4769(9) 0.9985(7) 0.1679(7) 0.045(3) Uani 1 1 d . . . . .
H58 H 0.4377 0.9667 0.1697 0.054 Uiso 1 1 calc R U . . .
C59 C 0.4659(12) 1.0682(9) 0.1081(10) 0.076(5) Uani 1 1 d . . . . .
H59A H 0.4915 1.1079 0.1158 0.115 Uiso 1 1 calc R U . . .
H59B H 0.3999 1.0983 0.1195 0.115 Uiso 1 1 calc R U . . .
H59C H 0.4992 1.0431 0.0506 0.115 Uiso 1 1 calc R U . . .
C60 C 0.4441(10) 1.0378(9) 0.2549(8) 0.056(3) Uani 1 1 d . . . . .
H60A H 0.4536 0.9928 0.2929 0.085 Uiso 1 1 calc R U . . .
H60B H 0.3780 1.0738 0.2747 0.085 Uiso 1 1 calc R U . . .
H60C H 0.4796 1.0720 0.2532 0.085 Uiso 1 1 calc R U . . .
C61 C 0.4601(7) 0.7884(6) 0.2221(6) 0.033(2) Uani 1 1 d . . . . .
H61 H 0.4817 0.7723 0.1646 0.039 Uiso 1 1 calc R U . . .
C62 C 0.3743(8) 0.7930(7) 0.2749(7) 0.039(2) Uani 1 1 d . . . . .
H62 H 0.3359 0.7803 0.2548 0.047 Uiso 1 1 calc R U . . .
C63 C 0.3435(7) 0.8164(7) 0.3579(7) 0.038(2) Uani 1 1 d . . . . .
H63 H 0.2829 0.8209 0.3953 0.046 Uiso 1 1 calc R U . . .
C64 C 0.3999(7) 0.8334(6) 0.3874(6) 0.035(2) Uani 1 1 d . . . . .
H64 H 0.3792 0.8490 0.4448 0.042 Uiso 1 1 calc R U . . .
C65 C 0.4863(7) 0.8272(6) 0.3317(6) 0.0302(19) Uani 1 1 d . . . . .
C66 C 0.5530(7) 0.8453(6) 0.3569(6) 0.0296(19) Uani 1 1 d . . . . .
H66A H 0.5370 0.9071 0.3613 0.036 Uiso 1 1 calc R U . . .
H66B H 0.5495 0.8233 0.4119 0.036 Uiso 1 1 calc R U . . .
C67 C 0.7197(7) 0.7759(6) 0.3133(6) 0.031(2) Uani 1 1 d . . . . .
C68 C 0.8922(7) 0.7083(7) 0.2461(6) 0.036(2) Uani 1 1 d . . . . .
C69 C 0.9619(8) 0.6307(8) 0.2155(7) 0.045(3) Uani 1 1 d . . . . .
H69 H 0.9474 0.5851 0.2059 0.054 Uiso 1 1 calc R U . . .
C70 C 1.0531(8) 0.6178(8) 0.1984(8) 0.053(3) Uani 1 1 d . . . . .
H70 H 1.1001 0.5631 0.1786 0.064 Uiso 1 1 calc R U . . .
C71 C 1.0772(8) 0.6847(8) 0.2099(7) 0.050(3) Uani 1 1 d . . . . .
C72 C 1.0069(8) 0.7614(8) 0.2417(7) 0.043(2) Uani 1 1 d . . . . .
H72 H 1.0210 0.8061 0.2543 0.051 Uiso 1 1 calc R U . . .
C73 C 0.9146(8) 0.7764(7) 0.2562(7) 0.042(2) Uani 1 1 d . . . . .
H73 H 0.8681 0.8317 0.2727 0.050 Uiso 1 1 calc R U . . .
C74 C 1.1759(9) 0.6696(10) 0.1959(9) 0.066(4) Uani 1 1 d . . . . .
H74A H 1.1894 0.7198 0.1738 0.099 Uiso 1 1 calc R U . . .
H74B H 1.2187 0.6207 0.1558 0.099 Uiso 1 1 calc R U . . .
H74C H 1.1834 0.6587 0.2489 0.099 Uiso 1 1 calc R U . . .
C75 C 0.7719(7) 0.7607(6) 0.4300(6) 0.031(2) Uani 1 1 d . . . . .
C76 C 0.8077(8) 0.6737(7) 0.4319(7) 0.044(3) Uani 1 1 d . . . . .
H76 H 0.7930 0.6385 0.4053 0.053 Uiso 1 1 calc R U . . .
C77 C 0.8657(10) 0.6397(9) 0.4738(8) 0.058(3) Uani 1 1 d . . . . .
H77 H 0.8905 0.5799 0.4759 0.070 Uiso 1 1 calc R U . . .
C78 C 0.8888(11) 0.6885(11) 0.5123(9) 0.067(4) Uani 1 1 d . . . . .
C79 C 0.8477(10) 0.7734(9) 0.5150(8) 0.058(3) Uani 1 1 d . . . . .
H79 H 0.8578 0.8081 0.5465 0.070 Uiso 1 1 calc R U . . .
C80 C 0.7907(9) 0.8109(8) 0.4724(7) 0.047(3) Uani 1 1 d . . . . .
H80 H 0.7647 0.8708 0.4723 0.057 Uiso 1 1 calc R U . . .
C81 C 0.9555(15) 0.6488(15) 0.5566(14) 0.116(8) Uani 1 1 d . . . . .
H81A H 0.9663 0.6935 0.5772 0.175 Uiso 1 1 calc R U . . .
H81B H 1.0147 0.6090 0.5171 0.175 Uiso 1 1 calc R U . . .
H81C H 0.9282 0.6186 0.6036 0.175 Uiso 1 1 calc R U . . .
C82 C 0.6944(7) 0.6871(7) 0.1580(6) 0.035(2) Uani 1 1 d . . . . .
Sb1 Sb 0.70328(6) 0.12154(5) 0.93075(5) 0.04475(19) Uani 1 1 d . . . . .
F1 F 0.7479(9) 0.0132(7) 0.9596(9) 0.125(5) Uani 1 1 d . . . . .
F2 F 0.6600(9) 0.2316(6) 0.9001(10) 0.124(5) Uani 1 1 d . . . . .
F3 F 0.7985(5) 0.1435(5) 0.9419(5) 0.063(2) Uani 1 1 d . . . . .
F4 F 0.6082(6) 0.1029(5) 0.9176(5) 0.063(2) Uani 1 1 d . . . . .
F5 F 0.6292(8) 0.1591(11) 1.0398(7) 0.149(7) Uani 1 1 d . . . . .
F6 F 0.7767(8) 0.0886(8) 0.8195(6) 0.108(4) Uani 1 1 d . . . . .
Sb2 Sb 0.66659(6) 0.05219(4) 0.36124(5) 0.0450(2) Uani 1 1 d . . . . .
F7 F 0.6003(5) -0.0168(4) 0.4185(6) 0.066(2) Uani 1 1 d . . . . .
F8 F 0.7360(6) 0.1182(4) 0.3063(5) 0.063(2) Uani 1 1 d . . . . .
F9 F 0.7384(6) 0.0122(5) 0.4234(5) 0.062(2) Uani 1 1 d . . . . .
F10 F 0.5966(6) 0.0930(5) 0.2974(5) 0.066(2) Uani 1 1 d . . . . .
F11 F 0.5801(6) 0.1412(4) 0.4427(4) 0.059(2) Uani 1 1 d . . . . .
F12 F 0.7483(6) -0.0376(4) 0.2796(5) 0.060(2) Uani 1 1 d . . . . .
Sb3 Sb 0.32569(5) 0.38227(4) 0.05412(4) 0.03089(15) Uani 1 1 d . . . . .
F13 F 0.3439(8) 0.2747(5) 0.0942(6) 0.082(3) Uani 1 1 d . . . . .
F14 F 0.3058(9) 0.4880(6) 0.0135(6) 0.098(4) Uani 1 1 d . . . . .
F15 F 0.2555(5) 0.4292(5) 0.1629(4) 0.061(2) Uani 1 1 d . . . . .
F16 F 0.3982(6) 0.3339(7) -0.0543(5) 0.085(3) Uani 1 1 d . . . . .
F17 F 0.4305(5) 0.3813(6) 0.0656(5) 0.070(2) Uani 1 1 d . . . . .
F18 F 0.2224(5) 0.3795(5) 0.0422(4) 0.0570(19) Uani 1 1 d . . . . .
Sb4 Sb 0.59695(6) 0.58258(4) 0.40029(4) 0.03870(19) Uani 1 1 d . . . . .
F19 F 0.6303(6) 0.5307(4) 0.4874(4) 0.0558(19) Uani 1 1 d . . . . .
F20 F 0.5634(5) 0.6336(4) 0.3128(4) 0.0493(17) Uani 1 1 d . . . . .
F21 F 0.7181(6) 0.5702(5) 0.3356(5) 0.0608(19) Uani 1 1 d . . . . .
F22 F 0.4739(5) 0.5970(4) 0.4638(4) 0.0534(17) Uani 1 1 d . . . . .
F23 F 0.6183(5) 0.4771(4) 0.3560(4) 0.0420(14) Uani 1 1 d . . . . .
F24 F 0.5738(6) 0.6883(4) 0.4454(4) 0.0558(19) Uani 1 1 d . . . . .
C91 C 0.7945(13) 0.5271(14) 0.6512(14) 0.123(8) Uani 1 1 d D . . . .
H91A H 0.7990 0.5834 0.6461 0.147 Uiso 1 1 calc R U . . .
H91B H 0.7537 0.5242 0.7096 0.147 Uiso 1 1 calc R U . . .
Cl1 Cl 0.9046(5) 0.4491(4) 0.6288(4) 0.122(2) Uani 1 1 d D . . . .
Cl2 Cl 0.7442(4) 0.5163(4) 0.5850(4) 0.1108(17) Uani 1 1 d D . . . .
C92 C 0.032(2) 0.0066(12) 0.8538(12) 0.147(11) Uani 1 1 d D . . . .
H92A H -0.0141 0.0625 0.8820 0.176 Uiso 1 1 calc R U . . .
H92B H 0.0943 0.0051 0.8443 0.176 Uiso 1 1 calc R U . . .
Cl3 Cl 0.0090(7) -0.0772(4) 0.9233(9) 0.245(7) Uani 1 1 d D . . . .
Cl4 Cl 0.0278(6) -0.0043(5) 0.7520(7) 0.197(5) Uani 1 1 d D . . . .
C93 C 0.8698(12) 0.9187(11) 0.6965(10) 0.096(6) Uani 1 1 d D . . . .
H93A H 0.8704 0.9538 0.7379 0.115 Uiso 1 1 calc R U . . .
H93B H 0.9318 0.8727 0.6725 0.115 Uiso 1 1 calc R U . . .
Cl5 Cl 0.7853(5) 0.8739(6) 0.7475(6) 0.185(4) Uani 1 1 d D . . . .
Cl6 Cl 0.8486(5) 0.9796(4) 0.6189(4) 0.121(2) Uani 1 1 d D . . . .
C94 C 0.953(2) 0.4875(19) -0.0179(14) 0.068(8) Uani 0.5 1 d D . P . .
H94A H 0.8914 0.5289 -0.0136 0.081 Uiso 0.5 1 calc R U P . .
H94B H 0.9665 0.4353 -0.0490 0.081 Uiso 0.5 1 calc R U P . .
Cl7 Cl 0.9504(4) 0.4650(4) 0.0788(3) 0.122(2) Uani 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C32 1.890(10) . ?
Os1 N1 2.077(8) . ?
Os1 N2 2.098(7) . ?
Os1 C3 2.219(8) . ?
Os1 C6 2.223(9) . ?
Os1 C2 2.232(9) . ?
Os1 C1 2.284(10) . ?
Os1 C5 2.299(8) . ?
Os1 C4 2.326(9) . ?
O1 C32 1.139(12) . ?
N1 C15 1.363(12) . ?
N1 C11 1.371(11) . ?
N2 C17 1.311(12) . ?
N2 C16 1.446(14) . ?
N3 C17 1.350(15) . ?
N3 C18 1.413(15) . ?
N3 H3N 0.84(13) . ?
N4 C17 1.366(13) . ?
N4 C25 1.427(12) . ?
N4 H4N 0.87(2) . ?
C1 C2 1.406(14) . ?
C1 C6 1.413(13) . ?
C1 C7 1.489(16) . ?
C2 C3 1.395(15) . ?
C2 H2 0.9500 . ?
C3 C4 1.448(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.405(13) . ?
C4 C8 1.500(14) . ?
C5 C6 1.438(15) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.514(14) . ?
C8 C10 1.528(16) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.351(15) . ?
C11 H11 0.9500 . ?
C12 C13 1.380(14) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.359(15) . ?
C14 H14 0.9500 . ?
C15 C16 1.501(13) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 C19 1.321(19) . ?
C18 C23 1.405(19) . ?
C19 C20 1.50(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.31(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.32(2) . ?
C21 C24 1.55(2) . ?
C22 C23 1.393(19) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C30 1.387(15) . ?
C25 C26 1.388(15) . ?
C26 C27 1.369(15) . ?
C26 H26 0.9500 . ?
C27 C28 1.369(17) . ?
C27 H27 0.9500 . ?
C28 C29 1.377(18) . ?
C28 C31 1.517(15) . ?
C29 C30 1.406(15) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
Os51 C82 1.904(11) . ?
Os51 N51 2.083(8) . ?
Os51 N52 2.100(7) . ?
Os51 C56 2.212(9) . ?
Os51 C53 2.220(9) . ?
Os51 C52 2.231(9) . ?
Os51 C51 2.278(11) . ?
Os51 C55 2.285(9) . ?
Os51 C54 2.329(10) . ?
O51 C82 1.134(12) . ?
N51 C65 1.345(12) . ?
N51 C61 1.372(11) . ?
N52 C67 1.320(12) . ?
N52 C66 1.462(13) . ?
N53 C67 1.346(14) . ?
N53 C68 1.411(13) . ?
N53 H53N 0.79(12) . ?
N54 C67 1.357(12) . ?
N54 C75 1.437(11) . ?
N54 H54N 0.95(11) . ?
C51 C52 1.418(15) . ?
C51 C56 1.433(16) . ?
C51 C57 1.54(2) . ?
C52 C53 1.395(16) . ?
C52 H52 0.9500 . ?
C53 C54 1.432(14) . ?
C53 H53 0.9500 . ?
C54 C55 1.415(15) . ?
C54 C58 1.474(17) . ?
C55 C56 1.436(17) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C60 1.520(17) . ?
C58 C59 1.520(16) . ?
C58 H58 1.0000 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.354(15) . ?
C61 H61 0.9500 . ?
C62 C63 1.375(15) . ?
C62 H62 0.9500 . ?
C63 C64 1.380(14) . ?
C63 H63 0.9500 . ?
C64 C65 1.369(14) . ?
C64 H64 0.9500 . ?
C65 C66 1.505(13) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C68 C69 1.370(15) . ?
C68 C73 1.402(15) . ?
C69 C70 1.384(16) . ?
C69 H69 0.9500 . ?
C70 C71 1.410(18) . ?
C70 H70 0.9500 . ?
C71 C72 1.367(17) . ?
C71 C74 1.511(17) . ?
C72 C73 1.405(16) . ?
C72 H72 0.9500 . ?
C73 H73 0.9500 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 C76 1.381(14) . ?
C75 C80 1.381(14) . ?
C76 C77 1.381(16) . ?
C76 H76 0.9500 . ?
C77 C78 1.37(2) . ?
C77 H77 0.9500 . ?
C78 C79 1.35(2) . ?
C78 C81 1.538(18) . ?
C79 C80 1.385(15) . ?
C79 H79 0.9500 . ?
C80 H80 0.9500 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
Sb1 F1 1.826(9) . ?
Sb1 F5 1.826(10) . ?
Sb1 F6 1.843(9) . ?
Sb1 F2 1.859(9) . ?
Sb1 F4 1.861(7) . ?
Sb1 F3 1.877(7) . ?
Sb2 F9 1.853(6) . ?
Sb2 F10 1.855(7) . ?
Sb2 F8 1.872(7) . ?
Sb2 F12 1.877(7) . ?
Sb2 F11 1.880(7) . ?
Sb2 F7 1.888(7) . ?
Sb3 F14 1.841(7) . ?
Sb3 F15 1.854(7) . ?
Sb3 F16 1.858(7) . ?
Sb3 F17 1.863(7) . ?
Sb3 F18 1.866(6) . ?
Sb3 F13 1.867(7) . ?
Sb4 F21 1.847(9) . ?
Sb4 F22 1.860(8) . ?
Sb4 F19 1.870(6) . ?
Sb4 F20 1.874(6) . ?
Sb4 F24 1.878(6) . ?
Sb4 F23 1.879(5) . ?
C91 Cl1 1.742(16) . ?
C91 Cl2 1.749(15) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 Cl4 1.845(16) . ?
C92 Cl3 1.851(17) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C93 Cl6 1.707(14) . ?
C93 Cl5 1.770(15) . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
C94 Cl7 1.690(16) . ?
C94 Cl7 1.99(3) 2_765 ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
Cl7 C94 1.99(3) 2_765 ?

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
C32 Os1 N1 88.6(4) . . ?
C32 Os1 N2 93.3(3) . . ?
N1 Os1 N2 77.1(3) . . ?
C32 Os1 C3 114.2(4) . . ?
N1 Os1 C3 94.9(3) . . ?
N2 Os1 C3 151.4(3) . . ?
C32 Os1 C6 121.1(4) . . ?
N1 Os1 C6 149.9(3) . . ?
N2 Os1 C6 94.7(3) . . ?
C3 Os1 C6 78.4(3) . . ?
C32 Os1 C2 91.0(4) . . ?
N1 Os1 C2 123.9(3) . . ?
N2 Os1 C2 158.7(4) . . ?
C3 Os1 C2 36.5(4) . . ?
C6 Os1 C2 65.4(3) . . ?
C32 Os1 C1 93.5(4) . . ?
N1 Os1 C1 160.1(3) . . ?
N2 Os1 C1 122.5(4) . . ?
C3 Os1 C1 66.2(4) . . ?
C6 Os1 C1 36.5(3) . . ?
C2 Os1 C1 36.3(4) . . ?
C32 Os1 C5 157.9(4) . . ?
N1 Os1 C5 113.5(3) . . ?
N2 Os1 C5 92.5(3) . . ?
C3 Os1 C5 65.2(3) . . ?
C6 Os1 C5 37.1(4) . . ?
C2 Os1 C5 76.3(3) . . ?
C1 Os1 C5 65.5(3) . . ?
C32 Os1 C4 151.1(4) . . ?
N1 Os1 C4 91.0(3) . . ?
N2 Os1 C4 114.8(3) . . ?
C3 Os1 C4 37.0(3) . . ?
C6 Os1 C4 65.9(3) . . ?
C2 Os1 C4 65.5(4) . . ?
C1 Os1 C4 77.6(3) . . ?
C5 Os1 C4 35.4(3) . . ?
C15 N1 C11 118.1(8) . . ?
C15 N1 Os1 117.8(6) . . ?
C11 N1 Os1 124.1(6) . . ?
C17 N2 C16 118.6(8) . . ?
C17 N2 Os1 127.6(8) . . ?
C16 N2 Os1 113.8(6) . . ?
C17 N3 C18 124.5(10) . . ?
C17 N3 H3N 130(9) . . ?
C18 N3 H3N 104(9) . . ?
C17 N4 C25 126.6(10) . . ?
C17 N4 H4N 107(8) . . ?
C25 N4 H4N 125(8) . . ?
C2 C1 C6 117.2(9) . . ?
C2 C1 C7 123.0(10) . . ?
C6 C1 C7 119.7(10) . . ?
C2 C1 Os1 69.9(6) . . ?
C6 C1 Os1 69.4(5) . . ?
C7 C1 Os1 129.8(7) . . ?
C3 C2 C1 122.6(9) . . ?
C3 C2 Os1 71.2(5) . . ?
C1 C2 Os1 73.9(5) . . ?
C3 C2 H2 118.7 . . ?
C1 C2 H2 118.7 . . ?
Os1 C2 H2 128.7 . . ?
C2 C3 C4 120.4(9) . . ?
C2 C3 Os1 72.2(5) . . ?
C4 C3 Os1 75.5(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
Os1 C3 H3 124.0 . . ?
C5 C4 C3 117.2(9) . . ?
C5 C4 C8 123.8(9) . . ?
C3 C4 C8 118.9(9) . . ?
C5 C4 Os1 71.2(5) . . ?
C3 C4 Os1 67.4(5) . . ?
C8 C4 Os1 130.3(6) . . ?
C4 C5 C6 121.0(8) . . ?
C4 C5 Os1 73.4(5) . . ?
C6 C5 Os1 68.6(5) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
Os1 C5 H5 131.3 . . ?
C1 C6 C5 120.9(9) . . ?
C1 C6 Os1 74.1(5) . . ?
C5 C6 Os1 74.3(5) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
Os1 C6 H6 123.4 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 C9 108.8(8) . . ?
C4 C8 C10 113.9(9) . . ?
C9 C8 C10 108.8(9) . . ?
C4 C8 H8 108.4 . . ?
C9 C8 H8 108.4 . . ?
C10 C8 H8 108.4 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N1 121.0(9) . . ?
C12 C11 H11 119.5 . . ?
N1 C11 H11 119.5 . . ?
C11 C12 C13 120.9(9) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 118.3(10) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C15 C14 C13 119.6(9) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 N1 122.1(9) . . ?
C14 C15 C16 123.5(9) . . ?
N1 C15 C16 114.4(9) . . ?
N2 C16 C15 110.4(8) . . ?
N2 C16 H16A 109.6 . . ?
C15 C16 H16A 109.6 . . ?
N2 C16 H16B 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
N2 C17 N3 120.9(9) . . ?
N2 C17 N4 120.6(11) . . ?
N3 C17 N4 118.5(9) . . ?
C19 C18 C23 119.2(14) . . ?
C19 C18 N3 119.7(14) . . ?
C23 C18 N3 121.1(12) . . ?
C18 C19 C20 118.3(16) . . ?
C18 C19 H19 120.9 . . ?
C20 C19 H19 120.9 . . ?
C21 C20 C19 118.9(17) . . ?
C21 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C20 C21 C22 123.3(18) . . ?
C20 C21 C24 115.0(17) . . ?
C22 C21 C24 121.7(19) . . ?
C21 C22 C23 119.2(16) . . ?
C21 C22 H22 120.4 . . ?
C23 C22 H22 120.4 . . ?
C22 C23 C18 121.0(15) . . ?
C22 C23 H23 119.5 . . ?
C18 C23 H23 119.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 120.2(10) . . ?
C30 C25 N4 117.0(10) . . ?
C26 C25 N4 122.7(9) . . ?
C27 C26 C25 119.5(11) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C26 122.4(12) . . ?
C28 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
C27 C28 C29 117.8(10) . . ?
C27 C28 C31 122.7(12) . . ?
C29 C28 C31 119.5(11) . . ?
C28 C29 C30 122.0(11) . . ?
C28 C29 H29 119.0 . . ?
C30 C29 H29 119.0 . . ?
C25 C30 C29 118.0(11) . . ?
C25 C30 H30 121.0 . . ?
C29 C30 H30 121.0 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O1 C32 Os1 177.0(10) . . ?
C82 Os51 N51 89.6(4) . . ?
C82 Os51 N52 92.6(3) . . ?
N51 Os51 N52 76.7(3) . . ?
C82 Os51 C56 123.4(5) . . ?
N51 Os51 C56 145.9(4) . . ?
N52 Os51 C56 92.1(3) . . ?
C82 Os51 C53 114.1(4) . . ?
N51 Os51 C53 96.2(3) . . ?
N52 Os51 C53 152.5(3) . . ?
C56 Os51 C53 78.9(4) . . ?
C82 Os51 C52 91.9(4) . . ?
N51 Os51 C52 126.6(4) . . ?
N52 Os51 C52 156.2(4) . . ?
C56 Os51 C52 66.2(4) . . ?
C53 Os51 C52 36.5(4) . . ?
C82 Os51 C51 95.1(5) . . ?
N51 Os51 C51 162.6(4) . . ?
N52 Os51 C51 119.7(4) . . ?
C56 Os51 C51 37.2(4) . . ?
C53 Os51 C51 66.6(4) . . ?
C52 Os51 C51 36.6(4) . . ?
C82 Os51 C55 160.2(5) . . ?
N51 Os51 C55 110.2(4) . . ?
N52 Os51 C55 92.2(3) . . ?
C56 Os51 C55 37.2(4) . . ?
C53 Os51 C55 65.0(3) . . ?
C52 Os51 C55 76.4(4) . . ?
C51 Os51 C55 66.0(5) . . ?
C82 Os51 C54 150.2(4) . . ?
N51 Os51 C54 89.3(3) . . ?
N52 Os51 C54 116.1(3) . . ?
C56 Os51 C54 66.6(4) . . ?
C53 Os51 C54 36.6(3) . . ?
C52 Os51 C54 65.4(4) . . ?
C51 Os51 C54 78.3(4) . . ?
C55 Os51 C54 35.7(4) . . ?
C65 N51 C61 119.0(8) . . ?
C65 N51 Os51 116.6(6) . . ?
C61 N51 Os51 124.4(6) . . ?
C67 N52 C66 121.0(7) . . ?
C67 N52 Os51 127.2(7) . . ?
C66 N52 Os51 111.5(5) . . ?
C67 N53 C68 129.4(9) . . ?
C67 N53 H53N 113(9) . . ?
C68 N53 H53N 117(9) . . ?
C67 N54 C75 126.4(9) . . ?
C67 N54 H54N 113(7) . . ?
C75 N54 H54N 119(7) . . ?
C52 C51 C56 116.6(11) . . ?
C52 C51 C57 121.2(11) . . ?
C56 C51 C57 122.0(11) . . ?
C52 C51 Os51 69.9(6) . . ?
C56 C51 Os51 68.9(6) . . ?
C57 C51 Os51 127.8(10) . . ?
C53 C52 C51 122.8(10) . . ?
C53 C52 Os51 71.3(5) . . ?
C51 C52 Os51 73.5(6) . . ?
C53 C52 H52 118.6 . . ?
C51 C52 H52 118.6 . . ?
Os51 C52 H52 129.2 . . ?
C52 C53 C54 121.4(9) . . ?
C52 C53 Os51 72.2(5) . . ?
C54 C53 Os51 75.9(5) . . ?
C52 C53 H53 119.3 . . ?
C54 C53 H53 119.3 . . ?
Os51 C53 H53 124.2 . . ?
C55 C54 C53 116.4(11) . . ?
C55 C54 C58 123.5(10) . . ?
C53 C54 C58 119.9(10) . . ?
C55 C54 Os51 70.4(6) . . ?
C53 C54 Os51 67.6(5) . . ?
C58 C54 Os51 129.9(7) . . ?
C54 C55 C56 122.1(10) . . ?
C54 C55 Os51 73.8(5) . . ?
C56 C55 Os51 68.7(6) . . ?
C54 C55 H55 118.9 . . ?
C56 C55 H55 118.9 . . ?
Os51 C55 H55 131.6 . . ?
C51 C56 C55 120.0(10) . . ?
C51 C56 Os51 73.9(6) . . ?
C55 C56 Os51 74.2(5) . . ?
C51 C56 H56 120.0 . . ?
C55 C56 H56 120.0 . . ?
Os51 C56 H56 123.4 . . ?
C51 C57 H57A 109.5 . . ?
C51 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C51 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C54 C58 C60 113.5(10) . . ?
C54 C58 C59 107.3(11) . . ?
C60 C58 C59 109.5(10) . . ?
C54 C58 H58 108.8 . . ?
C60 C58 H58 108.8 . . ?
C59 C58 H58 108.8 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 N51 121.2(9) . . ?
C62 C61 H61 119.4 . . ?
N51 C61 H61 119.4 . . ?
C61 C62 C63 119.1(9) . . ?
C61 C62 H62 120.4 . . ?
C63 C62 H62 120.4 . . ?
C62 C63 C64 120.5(10) . . ?
C62 C63 H63 119.8 . . ?
C64 C63 H63 119.8 . . ?
C65 C64 C63 118.2(9) . . ?
C65 C64 H64 120.9 . . ?
C63 C64 H64 120.9 . . ?
N51 C65 C64 121.9(9) . . ?
N51 C65 C66 115.4(8) . . ?
C64 C65 C66 122.6(8) . . ?
N52 C66 C65 108.3(7) . . ?
N52 C66 H66A 110.0 . . ?
C65 C66 H66A 110.0 . . ?
N52 C66 H66B 110.0 . . ?
C65 C66 H66B 110.0 . . ?
H66A C66 H66B 108.4 . . ?
N52 C67 N53 119.7(8) . . ?
N52 C67 N54 119.7(9) . . ?
N53 C67 N54 120.6(9) . . ?
C69 C68 C73 119.2(10) . . ?
C69 C68 N53 119.1(10) . . ?
C73 C68 N53 121.5(10) . . ?
C68 C69 C70 120.9(11) . . ?
C68 C69 H69 119.5 . . ?
C70 C69 H69 119.5 . . ?
C69 C70 C71 120.9(11) . . ?
C69 C70 H70 119.5 . . ?
C71 C70 H70 119.5 . . ?
C72 C71 C70 117.5(11) . . ?
C72 C71 C74 121.2(12) . . ?
C70 C71 C74 121.0(12) . . ?
C71 C72 C73 122.1(11) . . ?
C71 C72 H72 119.0 . . ?
C73 C72 H72 119.0 . . ?
C68 C73 C72 118.9(11) . . ?
C68 C73 H73 120.5 . . ?
C72 C73 H73 120.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C76 C75 C80 120.1(9) . . ?
C76 C75 N54 122.1(9) . . ?
C80 C75 N54 117.7(9) . . ?
C75 C76 C77 117.7(11) . . ?
C75 C76 H76 121.2 . . ?
C77 C76 H76 121.2 . . ?
C78 C77 C76 122.7(13) . . ?
C78 C77 H77 118.6 . . ?
C76 C77 H77 118.6 . . ?
C79 C78 C77 118.5(12) . . ?
C79 C78 C81 119.8(15) . . ?
C77 C78 C81 121.6(16) . . ?
C78 C79 C80 121.0(12) . . ?
C78 C79 H79 119.5 . . ?
C80 C79 H79 119.5 . . ?
C75 C80 C79 119.7(12) . . ?
C75 C80 H80 120.2 . . ?
C79 C80 H80 120.2 . . ?
C78 C81 H81A 109.5 . . ?
C78 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C78 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
O51 C82 Os51 177.4(11) . . ?
F1 Sb1 F5 91.3(8) . . ?
F1 Sb1 F6 91.3(7) . . ?
F5 Sb1 F6 177.4(7) . . ?
F1 Sb1 F2 179.0(7) . . ?
F5 Sb1 F2 89.5(8) . . ?
F6 Sb1 F2 88.0(7) . . ?
F1 Sb1 F4 91.2(4) . . ?
F5 Sb1 F4 90.8(4) . . ?
F6 Sb1 F4 89.6(4) . . ?
F2 Sb1 F4 89.5(4) . . ?
F1 Sb1 F3 90.7(4) . . ?
F5 Sb1 F3 89.7(4) . . ?
F6 Sb1 F3 89.8(4) . . ?
F2 Sb1 F3 88.6(4) . . ?
F4 Sb1 F3 178.1(4) . . ?
F9 Sb2 F10 178.8(4) . . ?
F9 Sb2 F8 89.2(3) . . ?
F10 Sb2 F8 89.7(4) . . ?
F9 Sb2 F12 90.8(3) . . ?
F10 Sb2 F12 88.8(3) . . ?
F8 Sb2 F12 90.7(3) . . ?
F9 Sb2 F11 91.1(3) . . ?
F10 Sb2 F11 89.3(3) . . ?
F8 Sb2 F11 91.2(3) . . ?
F12 Sb2 F11 177.3(3) . . ?
F9 Sb2 F7 88.5(3) . . ?
F10 Sb2 F7 92.6(4) . . ?
F8 Sb2 F7 177.6(3) . . ?
F12 Sb2 F7 88.9(3) . . ?
F11 Sb2 F7 89.3(3) . . ?
F14 Sb3 F15 91.4(4) . . ?
F14 Sb3 F16 89.3(5) . . ?
F15 Sb3 F16 178.7(4) . . ?
F14 Sb3 F17 90.7(5) . . ?
F15 Sb3 F17 88.7(3) . . ?
F16 Sb3 F17 90.2(3) . . ?
F14 Sb3 F18 90.9(4) . . ?
F15 Sb3 F18 92.1(3) . . ?
F16 Sb3 F18 89.0(3) . . ?
F17 Sb3 F18 178.2(4) . . ?
F14 Sb3 F13 178.5(4) . . ?
F15 Sb3 F13 89.1(4) . . ?
F16 Sb3 F13 90.2(5) . . ?
F17 Sb3 F13 90.7(4) . . ?
F18 Sb3 F13 87.7(4) . . ?
F21 Sb4 F22 178.6(3) . . ?
F21 Sb4 F19 91.0(3) . . ?
F22 Sb4 F19 90.4(3) . . ?
F21 Sb4 F20 89.2(3) . . ?
F22 Sb4 F20 89.5(3) . . ?
F19 Sb4 F20 179.4(3) . . ?
F21 Sb4 F24 90.2(3) . . ?
F22 Sb4 F24 89.4(3) . . ?
F19 Sb4 F24 89.6(3) . . ?
F20 Sb4 F24 91.0(3) . . ?
F21 Sb4 F23 90.7(3) . . ?
F22 Sb4 F23 89.8(3) . . ?
F19 Sb4 F23 90.5(3) . . ?
F20 Sb4 F23 88.9(3) . . ?
F24 Sb4 F23 179.1(3) . . ?
Cl1 C91 Cl2 112.7(11) . . ?
Cl1 C91 H91A 109.1 . . ?
Cl2 C91 H91A 109.1 . . ?
Cl1 C91 H91B 109.1 . . ?
Cl2 C91 H91B 109.1 . . ?
H91A C91 H91B 107.8 . . ?
Cl4 C92 Cl3 113.2(11) . . ?
Cl4 C92 H92A 108.9 . . ?
Cl3 C92 H92A 108.9 . . ?
Cl4 C92 H92B 108.9 . . ?
Cl3 C92 H92B 108.9 . . ?
H92A C92 H92B 107.8 . . ?
Cl6 C93 Cl5 112.0(10) . . ?
Cl6 C93 H93A 109.2 . . ?
Cl5 C93 H93A 109.2 . . ?
Cl6 C93 H93B 109.2 . . ?
Cl5 C93 H93B 109.2 . . ?
H93A C93 H93B 107.9 . . ?
Cl7 C94 Cl7 110.0(13) . 2_765 ?
Cl7 C94 H94A 109.7 . . ?
Cl7 C94 H94A 109.7 2_765 . ?
Cl7 C94 H94B 109.7 . . ?
Cl7 C94 H94B 109.7 2_765 . ?
H94A C94 H94B 108.2 . . ?
C94 Cl7 C94 70.0(13) . 2_765 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 2.0(14) . . . . ?
C7 C1 C2 C3 179.4(9) . . . . ?
Os1 C1 C2 C3 54.3(8) . . . . ?
C6 C1 C2 Os1 -52.4(8) . . . . ?
C7 C1 C2 Os1 125.1(10) . . . . ?
C1 C2 C3 C4 5.0(13) . . . . ?
Os1 C2 C3 C4 60.5(7) . . . . ?
C1 C2 C3 Os1 -55.5(8) . . . . ?
C2 C3 C4 C5 -6.1(12) . . . . ?
Os1 C3 C4 C5 52.8(7) . . . . ?
C2 C3 C4 C8 176.4(8) . . . . ?
Os1 C3 C4 C8 -124.8(7) . . . . ?
C2 C3 C4 Os1 -58.8(7) . . . . ?
C3 C4 C5 C6 0.5(12) . . . . ?
C8 C4 C5 C6 177.9(8) . . . . ?
Os1 C4 C5 C6 51.4(7) . . . . ?
C3 C4 C5 Os1 -51.0(7) . . . . ?
C8 C4 C5 Os1 126.5(8) . . . . ?
C2 C1 C6 C5 -7.6(13) . . . . ?
C7 C1 C6 C5 174.9(9) . . . . ?
Os1 C1 C6 C5 -60.2(7) . . . . ?
C2 C1 C6 Os1 52.6(8) . . . . ?
C7 C1 C6 Os1 -124.9(9) . . . . ?
C4 C5 C6 C1 6.5(13) . . . . ?
Os1 C5 C6 C1 60.1(8) . . . . ?
C4 C5 C6 Os1 -53.6(7) . . . . ?
C5 C4 C8 C9 106.7(10) . . . . ?
C3 C4 C8 C9 -75.9(11) . . . . ?
Os1 C4 C8 C9 -159.8(8) . . . . ?
C5 C4 C8 C10 -14.8(13) . . . . ?
C3 C4 C8 C10 162.6(9) . . . . ?
Os1 C4 C8 C10 78.7(11) . . . . ?
C15 N1 C11 C12 1.4(14) . . . . ?
Os1 N1 C11 C12 -176.9(8) . . . . ?
N1 C11 C12 C13 -1.2(16) . . . . ?
C11 C12 C13 C14 -0.6(17) . . . . ?
C12 C13 C14 C15 2.1(16) . . . . ?
C13 C14 C15 N1 -1.8(15) . . . . ?
C13 C14 C15 C16 177.7(10) . . . . ?
C11 N1 C15 C14 0.1(14) . . . . ?
Os1 N1 C15 C14 178.6(7) . . . . ?
C11 N1 C15 C16 -179.5(8) . . . . ?
Os1 N1 C15 C16 -1.0(10) . . . . ?
C17 N2 C16 C15 -155.2(8) . . . . ?
Os1 N2 C16 C15 27.6(9) . . . . ?
C14 C15 C16 N2 163.1(9) . . . . ?
N1 C15 C16 N2 -17.3(11) . . . . ?
C16 N2 C17 N3 168.7(8) . . . . ?
Os1 N2 C17 N3 -14.6(13) . . . . ?
C16 N2 C17 N4 -12.9(12) . . . . ?
Os1 N2 C17 N4 163.8(6) . . . . ?
C18 N3 C17 N2 135.2(10) . . . . ?
C18 N3 C17 N4 -43.2(14) . . . . ?
C25 N4 C17 N2 158.8(9) . . . . ?
C25 N4 C17 N3 -22.8(14) . . . . ?
C17 N3 C18 C19 160.7(11) . . . . ?
C17 N3 C18 C23 -20.8(16) . . . . ?
C23 C18 C19 C20 0.1(19) . . . . ?
N3 C18 C19 C20 178.6(12) . . . . ?
C18 C19 C20 C21 -2(2) . . . . ?
C19 C20 C21 C22 3(3) . . . . ?
C19 C20 C21 C24 -175.0(14) . . . . ?
C20 C21 C22 C23 -1(3) . . . . ?
C24 C21 C22 C23 175.9(14) . . . . ?
C21 C22 C23 C18 0(2) . . . . ?
C19 C18 C23 C22 1.0(19) . . . . ?
N3 C18 C23 C22 -177.6(11) . . . . ?
C17 N4 C25 C30 143.6(11) . . . . ?
C17 N4 C25 C26 -39.4(15) . . . . ?
C30 C25 C26 C27 -0.5(16) . . . . ?
N4 C25 C26 C27 -177.4(10) . . . . ?
C25 C26 C27 C28 0.2(17) . . . . ?
C26 C27 C28 C29 0.4(17) . . . . ?
C26 C27 C28 C31 177.1(11) . . . . ?
C27 C28 C29 C30 -0.9(18) . . . . ?
C31 C28 C29 C30 -177.7(12) . . . . ?
C26 C25 C30 C29 0.0(17) . . . . ?
N4 C25 C30 C29 177.1(10) . . . . ?
C28 C29 C30 C25 0.7(18) . . . . ?
C56 C51 C52 C53 1.6(16) . . . . ?
C57 C51 C52 C53 176.7(11) . . . . ?
Os51 C51 C52 C53 53.9(9) . . . . ?
C56 C51 C52 Os51 -52.3(9) . . . . ?
C57 C51 C52 Os51 122.8(12) . . . . ?
C51 C52 C53 C54 5.4(15) . . . . ?
Os51 C52 C53 C54 60.2(8) . . . . ?
C51 C52 C53 Os51 -54.9(9) . . . . ?
C52 C53 C54 C55 -6.0(13) . . . . ?
Os51 C53 C54 C55 52.4(7) . . . . ?
C52 C53 C54 C58 177.2(9) . . . . ?
Os51 C53 C54 C58 -124.3(9) . . . . ?
C52 C53 C54 Os51 -58.5(8) . . . . ?
C53 C54 C55 C56 0.0(13) . . . . ?
C58 C54 C55 C56 176.6(9) . . . . ?
Os51 C54 C55 C56 51.0(8) . . . . ?
C53 C54 C55 Os51 -51.0(7) . . . . ?
C58 C54 C55 Os51 125.6(9) . . . . ?
C52 C51 C56 C55 -7.6(15) . . . . ?
C57 C51 C56 C55 177.4(11) . . . . ?
Os51 C51 C56 C55 -60.3(8) . . . . ?
C52 C51 C56 Os51 52.8(9) . . . . ?
C57 C51 C56 Os51 -122.3(12) . . . . ?
C54 C55 C56 C51 6.9(14) . . . . ?
Os51 C55 C56 C51 60.2(9) . . . . ?
C54 C55 C56 Os51 -53.3(8) . . . . ?
C55 C54 C58 C60 -22.1(14) . . . . ?
C53 C54 C58 C60 154.4(9) . . . . ?
Os51 C54 C58 C60 69.7(12) . . . . ?
C55 C54 C58 C59 99.1(12) . . . . ?
C53 C54 C58 C59 -84.4(12) . . . . ?
Os51 C54 C58 C59 -169.1(9) . . . . ?
C65 N51 C61 C62 1.8(13) . . . . ?
Os51 N51 C61 C62 -176.9(7) . . . . ?
N51 C61 C62 C63 0.0(15) . . . . ?
C61 C62 C63 C64 -1.2(16) . . . . ?
C62 C63 C64 C65 0.7(15) . . . . ?
C61 N51 C65 C64 -2.3(13) . . . . ?
Os51 N51 C65 C64 176.4(7) . . . . ?
C61 N51 C65 C66 179.4(8) . . . . ?
Os51 N51 C65 C66 -1.9(10) . . . . ?
C63 C64 C65 N51 1.1(14) . . . . ?
C63 C64 C65 C66 179.3(9) . . . . ?
C67 N52 C66 C65 -149.4(8) . . . . ?
Os51 N52 C66 C65 36.1(8) . . . . ?
N51 C65 C66 N52 -22.5(10) . . . . ?
C64 C65 C66 N52 159.2(9) . . . . ?
C66 N52 C67 N53 162.4(8) . . . . ?
Os51 N52 C67 N53 -23.9(12) . . . . ?
C66 N52 C67 N54 -15.5(13) . . . . ?
Os51 N52 C67 N54 158.1(6) . . . . ?
C68 N53 C67 N52 148.5(10) . . . . ?
C68 N53 C67 N54 -33.5(15) . . . . ?
C75 N54 C67 N52 159.1(9) . . . . ?
C75 N54 C67 N53 -18.9(14) . . . . ?
C67 N53 C68 C69 155.6(10) . . . . ?
C67 N53 C68 C73 -29.4(16) . . . . ?
C73 C68 C69 C70 3.2(17) . . . . ?
N53 C68 C69 C70 178.3(11) . . . . ?
C68 C69 C70 C71 -1.7(19) . . . . ?
C69 C70 C71 C72 2.5(18) . . . . ?
C69 C70 C71 C74 176.6(12) . . . . ?
C70 C71 C72 C73 -5.1(17) . . . . ?
C74 C71 C72 C73 -179.1(11) . . . . ?
C69 C68 C73 C72 -5.6(15) . . . . ?
N53 C68 C73 C72 179.4(9) . . . . ?
C71 C72 C73 C68 6.7(16) . . . . ?
C67 N54 C75 C76 -39.3(15) . . . . ?
C67 N54 C75 C80 143.1(10) . . . . ?
C80 C75 C76 C77 -3.1(17) . . . . ?
N54 C75 C76 C77 179.5(11) . . . . ?
C75 C76 C77 C78 0(2) . . . . ?
C76 C77 C78 C79 5(2) . . . . ?
C76 C77 C78 C81 -178.4(16) . . . . ?
C77 C78 C79 C80 -7(2) . . . . ?
C81 C78 C79 C80 176.9(15) . . . . ?
C76 C75 C80 C79 1.7(18) . . . . ?
N54 C75 C80 C79 179.3(11) . . . . ?
C78 C79 C80 C75 3(2) . . . . ?
Cl7 C94 Cl7 C94 0.001(1) 2_765 . . 2_765 ?

_refine_diff_density_max         8.616
_refine_diff_density_min         -2.513
_refine_diff_density_rms         0.286

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_PLAT971_cmpnd_8             
;
PROBLEM: Check Calcd Resid. Dens.  0.86A   From Os51            8.19 eA-3  
RESPONSE: 

At the end of the refinement, when convergence is achieved, several residual
density peaks higher than 1 e/A^3 are observed. They are close to heavy atoms
(Sb or Os) or solvent molecules. They have no chemical sense.

;
_vrf_PLAT973_cmpnd_8             
;
PROBLEM: Check Calcd Positive Resid. Density on      Os51       4.98 eA-3  
RESPONSE: 
At the end of the refinement, when convergence is achieved, several residual
density peaks higher than 1 e/A^3 are observed. They are close to heavy atoms
(Sb or Os) or solvent molecules. They have no chemical sense.
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
