# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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. 
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data_str0594
_database_code_depnum_ccdc_archive 'CCDC 1509602'
_audit_update_record             
;
2016-10-12 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_audit_creation_date             2016-10-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C21 H11 N O11 Os3 S'
_chemical_formula_sum            'C21 H11 N O11 Os3 S'
_chemical_formula_weight         1055.97
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.2041(8)
_cell_length_b                   10.8173(8)
_cell_length_c                   11.4433(9)
_cell_angle_alpha                76.5340(10)
_cell_angle_beta                 80.9300(10)
_cell_angle_gamma                81.6510(10)
_cell_volume                     1205.27(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5886
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.56
_shelx_estimated_absorpt_T_max   0.402
_shelx_estimated_absorpt_T_min   0.199
_exptl_absorpt_coefficient_mu    15.923
_exptl_absorpt_correction_T_max  0.4019
_exptl_absorpt_correction_T_min  0.386891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1749 before and 0.0284 after correction.
The Ratio of minimum to maximum transmission is 0.3869.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.910
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9301
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.817
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4405
_reflns_number_total             4660
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.474
_refine_diff_density_min         -1.565
_refine_diff_density_rms         0.213
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4660
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0260
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0181P)²+1.6735P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0593
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C15(H15A,H15B)
2.b Me refined with riding coordinates:
 C11(H11A,H11B,H11C)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C26(H26)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.25390(2) 0.10048(2) 0.10596(2) 0.01291(7) Uani 1 1 d . . . . .
Os2 Os 0.24639(2) 0.14537(2) 0.34961(2) 0.01006(7) Uani 1 1 d . . . . .
Os3 Os 0.41963(2) 0.33241(2) 0.32684(2) 0.01064(7) Uani 1 1 d . . . . .
S1 S 0.07605(16) 0.66307(14) 0.34257(15) 0.0208(3) Uani 1 1 d . . . . .
N1 N 0.2361(5) 0.4573(4) 0.3409(4) 0.0118(10) Uani 1 1 d . . . . .
C1 C 0.2986(6) 0.0921(6) -0.0603(6) 0.0183(13) Uani 1 1 d . . . . .
C2 C 0.0731(7) 0.0513(6) 0.1262(6) 0.0218(14) Uani 1 1 d . . . . .
C3 C 0.3246(6) -0.0693(6) 0.1546(5) 0.0187(13) Uani 1 1 d . . . . .
C4 C 0.1265(6) 0.0201(6) 0.3753(5) 0.0180(13) Uani 1 1 d . . . . .
C5 C 0.3955(6) 0.0117(5) 0.3705(5) 0.0140(12) Uani 1 1 d . . . . .
C6 C 0.2308(6) 0.1642(5) 0.5136(5) 0.0126(12) Uani 1 1 d . . . . .
C7 C 0.5754(6) 0.2161(5) 0.3223(5) 0.0155(12) Uani 1 1 d . . . . .
C8 C 0.4445(6) 0.3499(6) 0.4869(6) 0.0183(13) Uani 1 1 d . . . . .
C9 C 0.5087(6) 0.4692(6) 0.2238(5) 0.0180(13) Uani 1 1 d . . . . .
O1 O 0.3268(5) 0.0862(5) -0.1596(4) 0.0337(12) Uani 1 1 d . . . . .
O2 O -0.0296(5) 0.0175(5) 0.1368(5) 0.0320(12) Uani 1 1 d . . . . .
O3 O 0.3701(5) -0.1732(4) 0.1874(4) 0.0288(11) Uani 1 1 d . . . . .
O4 O 0.0561(5) -0.0591(4) 0.3964(4) 0.0269(11) Uani 1 1 d . . . . .
O5 O 0.4790(4) -0.0687(4) 0.3906(4) 0.0223(10) Uani 1 1 d . . . . .
O6 O 0.2124(4) 0.1747(4) 0.6119(4) 0.0222(10) Uani 1 1 d . . . . .
O7 O 0.6708(4) 0.1447(4) 0.3223(4) 0.0255(10) Uani 1 1 d . . . . .
O8 O 0.4597(5) 0.3628(4) 0.5809(4) 0.0278(11) Uani 1 1 d . . . . .
O9 O 0.5631(4) 0.5488(4) 0.1604(4) 0.0277(11) Uani 1 1 d . . . . .
C11 C 0.2055(8) 0.6906(6) -0.0194(7) 0.0325(17) Uani 1 1 d . . . . .
H11A H 0.1479 0.7476 -0.0751 0.049 Uiso 1 1 calc R . . . .
H11B H 0.2988 0.6905 -0.0567 0.049 Uiso 1 1 calc R . . . .
H11C H 0.1952 0.7208 0.0562 0.049 Uiso 1 1 calc R . . . .
C12 C 0.1665(6) 0.5576(5) 0.0070(5) 0.0181(13) Uani 1 1 d . . . . .
H12A H 0.0724 0.5562 0.0448 0.022 Uiso 1 1 calc R . . . .
H12B H 0.1762 0.5259 -0.0688 0.022 Uiso 1 1 calc R . . . .
C13 C 0.2591(5) 0.3524(5) 0.1078(5) 0.0122(11) Uani 1 1 d . . . . .
C14 C 0.3520(6) 0.2695(5) 0.1876(5) 0.0132(12) Uani 1 1 d . . . . .
C15 C 0.4336(6) 0.1863(6) 0.1055(6) 0.0170(13) Uani 1 1 d . . . . .
H15A H 0.5050 0.1258 0.1438 0.020 Uiso 1 1 calc R . . . .
H15B H 0.4686 0.2350 0.0249 0.020 Uiso 1 1 calc R . . . .
C20 C 0.0866(6) 0.2982(5) 0.3334(5) 0.0125(12) Uani 1 1 d . . . . .
C21 C -0.0478(6) 0.2886(6) 0.3288(5) 0.0169(13) Uani 1 1 d . . . . .
H21 H -0.0721 0.2076 0.3272 0.020 Uiso 1 1 calc R . . . .
C22 C -0.1483(5) 0.3918(5) 0.3265(5) 0.0144(12) Uani 1 1 d . . . . .
H22 H -0.2374 0.3786 0.3229 0.017 Uiso 1 1 calc R . . . .
C23 C -0.1210(6) 0.5118(6) 0.3294(6) 0.0205(13) Uani 1 1 d . . . . .
H23 H -0.1896 0.5814 0.3279 0.025 Uiso 1 1 calc R . . . .
C24 C 0.0095(6) 0.5275(6) 0.3345(5) 0.0174(13) Uani 1 1 d . . . . .
C25 C 0.1104(6) 0.4228(5) 0.3370(5) 0.0140(12) Uani 1 1 d . . . . .
C26 C 0.2299(6) 0.5779(6) 0.3443(5) 0.0161(12) Uani 1 1 d . . . . .
H26 H 0.3071 0.6159 0.3475 0.019 Uiso 1 1 calc R . . . .
O10 O 0.1907(4) 0.3034(4) 0.0529(4) 0.0151(9) Uani 1 1 d . . . . .
O11 O 0.2557(4) 0.4772(4) 0.0900(4) 0.0159(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 Os2 2.9271(4) . ?
Os1 C1 1.905(6) . ?
Os1 C2 1.957(7) . ?
Os1 C3 1.862(7) . ?
Os1 C15 2.171(6) . ?
Os1 O10 2.167(4) . ?
Os2 Os3 2.8168(3) . ?
Os2 C4 1.898(6) . ?
Os2 C5 1.944(6) . ?
Os2 C6 1.914(6) . ?
Os2 C14 2.244(5) . ?
Os2 C20 2.144(5) . ?
Os3 N1 2.152(5) . ?
Os3 C7 1.880(6) . ?
Os3 C8 1.944(6) . ?
Os3 C9 1.909(6) . ?
Os3 C14 2.114(6) . ?
S1 C24 1.730(6) . ?
S1 C26 1.702(6) . ?
N1 C25 1.398(7) . ?
N1 C26 1.306(7) . ?
C1 O1 1.142(7) . ?
C2 O2 1.140(8) . ?
C3 O3 1.152(7) . ?
C4 O4 1.156(7) . ?
C5 O5 1.134(7) . ?
C6 O6 1.140(7) . ?
C7 O7 1.152(7) . ?
C8 O8 1.153(7) . ?
C9 O9 1.139(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 C12 1.499(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 O11 1.465(7) . ?
C13 C14 1.477(8) . ?
C13 O10 1.251(7) . ?
C13 O11 1.314(7) . ?
C14 C15 1.522(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C20 C21 1.400(8) . ?
C20 C25 1.415(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.400(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.375(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.378(8) . ?
C24 C25 1.414(8) . ?
C26 H26 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Os1 Os2 165.55(18) . . ?
C1 Os1 C2 96.9(3) . . ?
C1 Os1 C15 92.2(2) . . ?
C1 Os1 O10 89.9(2) . . ?
C2 Os1 Os2 97.28(18) . . ?
C2 Os1 C15 167.4(2) . . ?
C2 Os1 O10 94.2(2) . . ?
C3 Os1 Os2 91.49(18) . . ?
C3 Os1 C1 91.1(3) . . ?
C3 Os1 C2 91.5(3) . . ?
C3 Os1 C15 97.0(2) . . ?
C3 Os1 O10 174.1(2) . . ?
C15 Os1 Os2 73.33(16) . . ?
O10 Os1 Os2 86.09(10) . . ?
O10 Os1 C15 77.14(19) . . ?
Os3 Os2 Os1 106.101(9) . . ?
C4 Os2 Os1 77.51(18) . . ?
C4 Os2 Os3 176.37(18) . . ?
C4 Os2 C5 90.4(2) . . ?
C4 Os2 C6 97.6(2) . . ?
C4 Os2 C14 135.8(2) . . ?
C4 Os2 C20 92.0(2) . . ?
C5 Os2 Os1 87.22(17) . . ?
C5 Os2 Os3 90.18(17) . . ?
C5 Os2 C14 95.0(2) . . ?
C5 Os2 C20 176.7(2) . . ?
C6 Os2 Os1 175.11(17) . . ?
C6 Os2 Os3 78.79(17) . . ?
C6 Os2 C5 92.9(2) . . ?
C6 Os2 C14 125.8(2) . . ?
C6 Os2 C20 84.5(2) . . ?
C14 Os2 Os1 59.01(14) . . ?
C14 Os2 Os3 47.74(14) . . ?
C20 Os2 Os1 95.61(15) . . ?
C20 Os2 Os3 87.32(15) . . ?
C20 Os2 C14 85.0(2) . . ?
N1 Os3 Os2 83.31(12) . . ?
C7 Os3 Os2 94.28(17) . . ?
C7 Os3 N1 176.6(2) . . ?
C7 Os3 C8 90.2(3) . . ?
C7 Os3 C9 92.5(2) . . ?
C7 Os3 C14 91.6(2) . . ?
C8 Os3 Os2 109.52(17) . . ?
C8 Os3 N1 88.3(2) . . ?
C8 Os3 C14 161.3(2) . . ?
C9 Os3 Os2 147.64(18) . . ?
C9 Os3 N1 90.8(2) . . ?
C9 Os3 C8 102.0(2) . . ?
C9 Os3 C14 96.5(2) . . ?
C14 Os3 Os2 51.77(15) . . ?
C14 Os3 N1 88.82(19) . . ?
C26 S1 C24 89.5(3) . . ?
C25 N1 Os3 124.3(4) . . ?
C26 N1 Os3 123.9(4) . . ?
C26 N1 C25 111.6(5) . . ?
O1 C1 Os1 179.1(6) . . ?
O2 C2 Os1 176.9(6) . . ?
O3 C3 Os1 177.9(5) . . ?
O4 C4 Os2 176.5(6) . . ?
O5 C5 Os2 175.4(5) . . ?
O6 C6 Os2 175.3(5) . . ?
O7 C7 Os3 178.4(5) . . ?
O8 C8 Os3 178.6(5) . . ?
O9 C9 Os3 178.2(6) . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
C11 C12 H12A 110.3 . . ?
C11 C12 H12B 110.3 . . ?
H12A C12 H12B 108.6 . . ?
O11 C12 C11 106.9(5) . . ?
O11 C12 H12A 110.3 . . ?
O11 C12 H12B 110.3 . . ?
O10 C13 C14 119.8(5) . . ?
O10 C13 O11 121.0(5) . . ?
O11 C13 C14 119.1(5) . . ?
Os3 C14 Os2 80.49(19) . . ?
C13 C14 Os2 112.7(4) . . ?
C13 C14 Os3 122.0(4) . . ?
C13 C14 C15 102.6(5) . . ?
C15 C14 Os2 109.6(4) . . ?
C15 C14 Os3 126.6(4) . . ?
Os1 C15 H15A 113.9 . . ?
Os1 C15 H15B 113.9 . . ?
C14 C15 Os1 88.4(3) . . ?
C14 C15 H15A 113.9 . . ?
C14 C15 H15B 113.9 . . ?
H15A C15 H15B 111.1 . . ?
C21 C20 Os2 127.1(4) . . ?
C21 C20 C25 113.0(5) . . ?
C25 C20 Os2 119.7(4) . . ?
C20 C21 H21 118.2 . . ?
C20 C21 C22 123.7(5) . . ?
C22 C21 H21 118.2 . . ?
C21 C22 H22 119.2 . . ?
C23 C22 C21 121.6(5) . . ?
C23 C22 H22 119.2 . . ?
C22 C23 H23 121.2 . . ?
C22 C23 C24 117.6(6) . . ?
C24 C23 H23 121.2 . . ?
C23 C24 S1 129.2(5) . . ?
C23 C24 C25 120.4(5) . . ?
C25 C24 S1 110.3(4) . . ?
N1 C25 C20 124.1(5) . . ?
N1 C25 C24 112.2(5) . . ?
C24 C25 C20 123.6(5) . . ?
S1 C26 H26 121.8 . . ?
N1 C26 S1 116.4(5) . . ?
N1 C26 H26 121.8 . . ?
C13 O10 Os1 103.2(3) . . ?
C13 O11 C12 118.2(4) . . ?

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
Os2 C14 C15 Os1 53.2(3) . . . . ?
Os2 C20 C21 C22 175.4(4) . . . . ?
Os2 C20 C25 N1 5.4(8) . . . . ?
Os2 C20 C25 C24 -175.9(4) . . . . ?
Os3 N1 C25 C20 5.4(8) . . . . ?
Os3 N1 C25 C24 -173.3(4) . . . . ?
Os3 N1 C26 S1 174.6(3) . . . . ?
Os3 C14 C15 Os1 145.8(4) . . . . ?
S1 C24 C25 N1 -2.1(6) . . . . ?
S1 C24 C25 C20 179.1(5) . . . . ?
C11 C12 O11 C13 -166.8(5) . . . . ?
C13 C14 C15 Os1 -66.8(4) . . . . ?
C14 C13 O10 Os1 -1.3(6) . . . . ?
C14 C13 O11 C12 177.8(5) . . . . ?
C20 C21 C22 C23 -0.4(9) . . . . ?
C21 C20 C25 N1 -179.5(5) . . . . ?
C21 C20 C25 C24 -0.8(8) . . . . ?
C21 C22 C23 C24 0.0(9) . . . . ?
C22 C23 C24 S1 -178.4(5) . . . . ?
C22 C23 C24 C25 -0.1(9) . . . . ?
C23 C24 C25 N1 179.3(5) . . . . ?
C23 C24 C25 C20 0.6(9) . . . . ?
C24 S1 C26 N1 -0.8(5) . . . . ?
C25 N1 C26 S1 -0.3(6) . . . . ?
C25 C20 C21 C22 0.8(8) . . . . ?
C26 S1 C24 C23 180.0(6) . . . . ?
C26 S1 C24 C25 1.6(5) . . . . ?
C26 N1 C25 C20 -179.7(5) . . . . ?
C26 N1 C25 C24 1.5(7) . . . . ?
O10 C13 C14 Os2 -65.6(6) . . . . ?
O10 C13 C14 Os3 -158.5(4) . . . . ?
O10 C13 C14 C15 52.2(6) . . . . ?
O10 C13 O11 C12 1.9(8) . . . . ?
O11 C13 C14 Os2 118.5(5) . . . . ?
O11 C13 C14 Os3 25.6(7) . . . . ?
O11 C13 C14 C15 -123.7(5) . . . . ?
O11 C13 O10 Os1 174.5(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_xstr0280
_database_code_depnum_ccdc_archive 'CCDC 1509600'
_audit_update_record             
;
2016-10-12 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_xstr0280            
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        6.2 Ratio
RESPONSE: This is the terminal C atom of an OEt group which is undergoung thermal vibration/
;
# Added during the CSD deposition process: Wednesday 12 October 2016 04:54 PM
# end Validation Reply Form

_audit_creation_date             2016-10-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H15 N O13 Os3 S'
_chemical_formula_sum            'C24 H15 N O13 Os3 S'
_chemical_formula_weight         1128.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Os3 C24 O13 H15 S1 N1'
_chemical_oxdiff_usercomment     AH-146C
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.2449(3)
_cell_length_b                   11.0705(4)
_cell_length_c                   13.4872(4)
_cell_angle_alpha                78.130(3)
_cell_angle_beta                 74.717(3)
_cell_angle_gamma                81.572(3)
_cell_volume                     1437.09(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11971
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      29.1140
_cell_measurement_theta_min      3.5080
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.369
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19242
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.899
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -44.00   39.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092  -57.0000   60.0000 83

#__ type_ start__ end____ width___ exp.time_
  2 omega  -16.00   52.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092  -99.0000  -30.0000 68

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   91.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092   19.0000  150.0000 116

#__ type_ start__ end____ width___ exp.time_
  4 omega  -19.00   57.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092   77.0000  -30.0000 76

#__ type_ start__ end____ width___ exp.time_
  5 omega  -13.00   85.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092   38.0000 -120.0000 98

#__ type_ start__ end____ width___ exp.time_
  6 omega  -59.00   44.00   1.0000    1.5750
omega____ theta____ kappa____ phi______ frames
    -       11.0092  -77.0000 -180.0000 103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0715527000
_diffrn_orient_matrix_UB_12      0.0015391000
_diffrn_orient_matrix_UB_13      -0.0162398000
_diffrn_orient_matrix_UB_21      0.0083241000
_diffrn_orient_matrix_UB_22      -0.0651075000
_diffrn_orient_matrix_UB_23      0.0018542000
_diffrn_orient_matrix_UB_31      -0.0034693000
_diffrn_orient_matrix_UB_32      0.0093005000
_diffrn_orient_matrix_UB_33      -0.0529066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5159
_reflns_number_total             5630
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         3.039
_refine_diff_density_min         -2.619
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       0.00116(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5630
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0348
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0451P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0862
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C14(H14), C15(H15)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.46612(2) 0.72275(2) 0.79723(2) 0.01409(10) Uani 1 1 d . . . . .
Os2 Os 0.67962(2) 0.82513(2) 0.63654(2) 0.01353(10) Uani 1 1 d . . . . .
Os3 Os 0.92079(3) 0.64735(2) 0.64210(2) 0.01515(10) Uani 1 1 d . . . . .
S1 S 0.5877(2) 0.85119(19) 1.06559(13) 0.0260(4) Uani 1 1 d . . . . .
O1 O 0.3399(5) 0.6624(5) 0.6354(4) 0.0296(12) Uani 1 1 d . . . . .
O2 O 0.3697(5) 0.4901(5) 0.9464(4) 0.0317(13) Uani 1 1 d . . . . .
O3 O 0.2250(5) 0.9222(5) 0.8430(4) 0.0331(13) Uani 1 1 d . . . . .
O4 O 0.4411(6) 1.0233(5) 0.6317(4) 0.0346(14) Uani 1 1 d . . . . .
O5 O 0.8709(6) 0.9937(6) 0.4732(4) 0.0392(14) Uani 1 1 d . . . . .
O6 O 0.6426(5) 0.7149(5) 0.4547(4) 0.0273(12) Uani 1 1 d . . . . .
O7 O 1.0346(6) 0.7397(6) 0.4068(4) 0.0394(15) Uani 1 1 d . . . . .
O8 O 1.0753(5) 0.8102(5) 0.7147(4) 0.0293(12) Uani 1 1 d . . . . .
O9 O 1.1423(6) 0.4394(6) 0.6772(5) 0.0400(15) Uani 1 1 d . . . . .
O10 O 0.7989(4) 0.5194(4) 0.6150(3) 0.0164(10) Uani 1 1 d . . . . .
O11 O 0.5784(5) 0.4914(4) 0.6670(3) 0.0177(10) Uani 1 1 d . . . . .
O12 O 0.8984(5) 0.4499(4) 0.8925(3) 0.0209(11) Uani 1 1 d . . . . .
O13 O 0.7329(5) 0.3918(5) 0.8382(4) 0.0247(11) Uani 1 1 d . . . . .
N1 N 0.5518(5) 0.7898(5) 0.9028(4) 0.0163(12) Uani 1 1 d . . . . .
C1 C 0.3908(7) 0.6820(7) 0.6964(5) 0.0210(16) Uani 1 1 d . . . . .
C2 C 0.4055(7) 0.5795(7) 0.8939(5) 0.0199(15) Uani 1 1 d . . . . .
C3 C 0.3125(7) 0.8468(6) 0.8262(5) 0.0175(14) Uani 1 1 d . . . . .
C4 C 0.5260(8) 0.9457(7) 0.6400(5) 0.0217(16) Uani 1 1 d . . . . .
C5 C 0.8034(8) 0.9302(7) 0.5364(5) 0.0241(16) Uani 1 1 d . . . . .
C6 C 0.6543(7) 0.7559(6) 0.5230(5) 0.0204(15) Uani 1 1 d . . . . .
C7 C 0.9956(7) 0.7039(7) 0.4932(6) 0.0217(15) Uani 1 1 d . . . . .
C8 C 1.0152(7) 0.7525(7) 0.6844(5) 0.0207(15) Uani 1 1 d . . . . .
C9 C 1.0574(7) 0.5161(7) 0.6638(5) 0.0209(15) Uani 1 1 d . . . . .
C10 C 0.5082(7) 0.7741(7) 1.0038(5) 0.0202(15) Uani 1 1 d . . . . .
H10 H 0.4389 0.7246 1.0400 0.024 Uiso 1 1 calc R . . . .
C11 C 0.6561(7) 0.8685(6) 0.8646(5) 0.0175(14) Uani 1 1 d . . . . .
C12 C 0.6876(8) 0.9139(7) 0.9452(5) 0.0224(16) Uani 1 1 d . . . . .
C13 C 0.7860(8) 0.9969(7) 0.9244(6) 0.0284(18) Uani 1 1 d . . . . .
H13 H 0.8093 1.0249 0.9773 0.034 Uiso 1 1 calc R . . . .
C14 C 0.8453(7) 1.0341(7) 0.8219(6) 0.0247(16) Uani 1 1 d . . . . .
H14 H 0.9079 1.0926 0.8041 0.030 Uiso 1 1 calc R . . . .
C15 C 0.8155(7) 0.9875(6) 0.7417(5) 0.0205(15) Uani 1 1 d . . . . .
H15 H 0.8606 1.0162 0.6732 0.025 Uiso 1 1 calc R . . . .
C16 C 0.7224(7) 0.9007(6) 0.7586(5) 0.0162(14) Uani 1 1 d . . . . .
C17 C 0.6212(9) 0.2722(7) 0.6544(6) 0.036(2) Uani 1 1 d . . . . .
H17A H 0.6404 0.2145 0.6069 0.054 Uiso 1 1 calc GR . . . .
H17B H 0.5400 0.2535 0.7074 0.054 Uiso 1 1 calc GR . . . .
H17C H 0.6958 0.2657 0.6864 0.054 Uiso 1 1 calc GR . . . .
C18 C 0.6014(8) 0.4009(7) 0.5962(5) 0.0246(16) Uani 1 1 d . . . . .
H18A H 0.6812 0.4181 0.5398 0.030 Uiso 1 1 calc R . . . .
H18B H 0.5239 0.4085 0.5659 0.030 Uiso 1 1 calc R . . . .
C19 C 0.6831(7) 0.5432(6) 0.6706(5) 0.0158(14) Uani 1 1 d . . . . .
C20 C 0.6620(6) 0.6362(5) 0.7400(5) 0.0118(13) Uani 1 1 d . . . . .
C21 C 0.7801(6) 0.6019(6) 0.7934(5) 0.0124(13) Uani 1 1 d . . . . .
H21 H 0.7795 0.6589 0.8404 0.015 Uiso 1 1 calc R . . . .
C22 C 0.7981(6) 0.4719(6) 0.8425(5) 0.0147(14) Uani 1 1 d . . . . .
C23 C 0.9289(8) 0.3223(7) 0.9405(6) 0.0293(18) Uani 1 1 d . . . . .
H23A H 0.8457 0.2881 0.9823 0.035 Uiso 1 1 calc R . . . .
H23B H 0.9702 0.2725 0.8870 0.035 Uiso 1 1 calc R . . . .
C24 C 1.0213(13) 0.3200(10) 1.0060(9) 0.072(4) Uani 1 1 d . . . . .
H24A H 1.1051 0.3501 0.9637 0.108 Uiso 1 1 calc GR . . . .
H24B H 1.0390 0.2365 1.0404 0.108 Uiso 1 1 calc GR . . . .
H24C H 0.9811 0.3719 1.0573 0.108 Uiso 1 1 calc GR . . . .


_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 Os2 2.8254(4) . ?
Os1 N1 2.153(5) . ?
Os1 C1 1.885(7) . ?
Os1 C2 1.901(7) . ?
Os1 C3 1.944(7) . ?
Os1 C20 2.113(6) . ?
Os2 Os3 2.9318(4) . ?
Os2 C4 1.906(8) . ?
Os2 C5 1.915(8) . ?
Os2 C6 1.936(8) . ?
Os2 C16 2.158(7) . ?
Os2 C20 2.265(6) . ?
Os3 O10 2.161(5) . ?
Os3 C7 1.955(7) . ?
Os3 C8 1.874(8) . ?
Os3 C9 1.898(8) . ?
Os3 C21 2.176(6) . ?
S1 C10 1.714(7) . ?
S1 C12 1.742(8) . ?
O1 C1 1.153(8) . ?
O2 C2 1.138(8) . ?
O3 C3 1.142(8) . ?
O4 C4 1.140(9) . ?
O5 C5 1.133(9) . ?
O6 C6 1.148(8) . ?
O7 C7 1.134(8) . ?
O8 C8 1.144(9) . ?
O9 C9 1.147(9) . ?
O10 C19 1.249(8) . ?
O11 C18 1.476(8) . ?
O11 C19 1.304(8) . ?
O12 C22 1.340(8) . ?
O12 C23 1.454(8) . ?
O13 C22 1.205(8) . ?
N1 C10 1.300(8) . ?
N1 C11 1.401(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.412(10) . ?
C11 C16 1.408(9) . ?
C12 C13 1.398(11) . ?
C13 H13 0.9300 . ?
C13 C14 1.359(10) . ?
C14 H14 0.9300 . ?
C14 C15 1.407(9) . ?
C15 H15 0.9300 . ?
C15 C16 1.396(10) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 C18 1.492(11) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.486(9) . ?
C20 C21 1.529(8) . ?
C21 H21 0.9800 . ?
C21 C22 1.462(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.450(12) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Os1 Os2 86.41(15) . . ?
C1 Os1 Os2 89.8(2) . . ?
C1 Os1 N1 173.7(3) . . ?
C1 Os1 C2 91.3(3) . . ?
C1 Os1 C3 88.8(3) . . ?
C1 Os1 C20 94.5(3) . . ?
C2 Os1 Os2 146.5(2) . . ?
C2 Os1 N1 94.7(3) . . ?
C2 Os1 C3 102.7(3) . . ?
C2 Os1 C20 94.3(3) . . ?
C3 Os1 Os2 110.79(19) . . ?
C3 Os1 N1 87.8(2) . . ?
C3 Os1 C20 162.5(3) . . ?
C20 Os1 Os2 52.20(16) . . ?
C20 Os1 N1 87.2(2) . . ?
Os1 Os2 Os3 106.246(11) . . ?
C4 Os2 Os1 73.6(2) . . ?
C4 Os2 Os3 176.0(2) . . ?
C4 Os2 C5 94.9(3) . . ?
C4 Os2 C6 95.5(3) . . ?
C4 Os2 C16 87.5(3) . . ?
C4 Os2 C20 120.9(3) . . ?
C5 Os2 Os1 166.7(2) . . ?
C5 Os2 Os3 84.8(2) . . ?
C5 Os2 C6 88.6(3) . . ?
C5 Os2 C16 88.7(3) . . ?
C5 Os2 C20 144.2(3) . . ?
C6 Os2 Os1 98.88(19) . . ?
C6 Os2 Os3 88.4(2) . . ?
C6 Os2 C16 176.1(3) . . ?
C6 Os2 C20 89.6(2) . . ?
C16 Os2 Os1 84.26(18) . . ?
C16 Os2 Os3 88.53(17) . . ?
C16 Os2 C20 90.9(2) . . ?
C20 Os2 Os1 47.49(15) . . ?
C20 Os2 Os3 59.43(16) . . ?
O10 Os3 Os2 84.45(12) . . ?
O10 Os3 C21 76.9(2) . . ?
C7 Os3 Os2 90.5(2) . . ?
C7 Os3 O10 93.5(2) . . ?
C7 Os3 C21 162.6(3) . . ?
C8 Os3 Os2 94.8(2) . . ?
C8 Os3 O10 172.4(2) . . ?
C8 Os3 C7 94.0(3) . . ?
C8 Os3 C9 89.2(3) . . ?
C8 Os3 C21 95.7(3) . . ?
C9 Os3 Os2 170.5(2) . . ?
C9 Os3 O10 90.4(2) . . ?
C9 Os3 C7 97.8(3) . . ?
C9 Os3 C21 96.8(3) . . ?
C21 Os3 Os2 74.36(16) . . ?
C10 S1 C12 89.9(3) . . ?
C19 O10 Os3 104.2(4) . . ?
C19 O11 C18 117.7(5) . . ?
C22 O12 C23 116.9(6) . . ?
C10 N1 Os1 126.2(5) . . ?
C10 N1 C11 112.9(6) . . ?
C11 N1 Os1 120.7(4) . . ?
O1 C1 Os1 176.5(6) . . ?
O2 C2 Os1 175.5(6) . . ?
O3 C3 Os1 178.0(6) . . ?
O4 C4 Os2 172.8(6) . . ?
O5 C5 Os2 175.6(6) . . ?
O6 C6 Os2 178.4(6) . . ?
O7 C7 Os3 177.4(6) . . ?
O8 C8 Os3 175.5(6) . . ?
O9 C9 Os3 177.9(7) . . ?
S1 C10 H10 122.4 . . ?
N1 C10 S1 115.2(6) . . ?
N1 C10 H10 122.4 . . ?
N1 C11 C12 112.2(6) . . ?
N1 C11 C16 124.8(6) . . ?
C16 C11 C12 123.0(7) . . ?
C11 C12 S1 109.8(6) . . ?
C13 C12 S1 128.4(6) . . ?
C13 C12 C11 121.8(7) . . ?
C12 C13 H13 122.2 . . ?
C14 C13 C12 115.7(7) . . ?
C14 C13 H13 122.2 . . ?
C13 C14 H14 118.8 . . ?
C13 C14 C15 122.5(7) . . ?
C15 C14 H14 118.8 . . ?
C14 C15 H15 118.0 . . ?
C16 C15 C14 124.0(7) . . ?
C16 C15 H15 118.0 . . ?
C11 C16 Os2 122.8(5) . . ?
C15 C16 Os2 124.3(5) . . ?
C15 C16 C11 112.8(6) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
O11 C18 C17 110.2(6) . . ?
O11 C18 H18A 109.6 . . ?
O11 C18 H18B 109.6 . . ?
C17 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
O10 C19 O11 121.7(6) . . ?
O10 C19 C20 119.6(6) . . ?
O11 C19 C20 118.7(6) . . ?
Os1 C20 Os2 80.31(19) . . ?
C19 C20 Os1 121.0(4) . . ?
C19 C20 Os2 107.3(4) . . ?
C19 C20 C21 104.1(5) . . ?
C21 C20 Os1 128.4(4) . . ?
C21 C20 Os2 110.5(4) . . ?
Os3 C21 H21 112.2 . . ?
C20 C21 Os3 89.1(4) . . ?
C20 C21 H21 112.2 . . ?
C22 C21 Os3 113.6(4) . . ?
C22 C21 C20 115.5(5) . . ?
C22 C21 H21 112.2 . . ?
O12 C22 C21 112.3(6) . . ?
O13 C22 O12 122.8(6) . . ?
O13 C22 C21 124.9(6) . . ?
O12 C23 H23A 109.9 . . ?
O12 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 O12 108.9(7) . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Os1 N1 C10 S1 -174.0(3) . . . . ?
Os1 N1 C11 C12 173.1(4) . . . . ?
Os1 N1 C11 C16 -6.4(9) . . . . ?
Os1 C20 C21 Os3 -144.3(4) . . . . ?
Os1 C20 C21 C22 99.8(6) . . . . ?
Os2 C20 C21 Os3 -50.5(3) . . . . ?
Os2 C20 C21 C22 -166.3(4) . . . . ?
Os3 O10 C19 O11 173.5(5) . . . . ?
Os3 O10 C19 C20 -4.2(6) . . . . ?
Os3 C21 C22 O12 82.4(6) . . . . ?
Os3 C21 C22 O13 -96.5(7) . . . . ?
S1 C12 C13 C14 -177.7(5) . . . . ?
O10 C19 C20 Os1 160.0(4) . . . . ?
O10 C19 C20 Os2 71.1(6) . . . . ?
O10 C19 C20 C21 -46.1(7) . . . . ?
O11 C19 C20 Os1 -17.7(7) . . . . ?
O11 C19 C20 Os2 -106.7(5) . . . . ?
O11 C19 C20 C21 136.2(5) . . . . ?
N1 C11 C12 S1 1.8(7) . . . . ?
N1 C11 C12 C13 -178.1(7) . . . . ?
N1 C11 C16 Os2 -3.2(9) . . . . ?
N1 C11 C16 C15 175.7(6) . . . . ?
C10 S1 C12 C11 -1.7(5) . . . . ?
C10 S1 C12 C13 178.3(7) . . . . ?
C10 N1 C11 C12 -1.0(8) . . . . ?
C10 N1 C11 C16 179.5(6) . . . . ?
C11 N1 C10 S1 -0.3(8) . . . . ?
C11 C12 C13 C14 2.3(11) . . . . ?
C12 S1 C10 N1 1.2(6) . . . . ?
C12 C11 C16 Os2 177.4(5) . . . . ?
C12 C11 C16 C15 -3.7(10) . . . . ?
C12 C13 C14 C15 -3.3(11) . . . . ?
C13 C14 C15 C16 0.8(12) . . . . ?
C14 C15 C16 Os2 -178.4(5) . . . . ?
C14 C15 C16 C11 2.7(10) . . . . ?
C16 C11 C12 S1 -178.7(5) . . . . ?
C16 C11 C12 C13 1.4(11) . . . . ?
C18 O11 C19 O10 1.2(9) . . . . ?
C18 O11 C19 C20 178.9(5) . . . . ?
C19 O11 C18 C17 95.4(7) . . . . ?
C19 C20 C21 Os3 64.5(4) . . . . ?
C19 C20 C21 C22 -51.4(7) . . . . ?
C20 C21 C22 O12 -176.6(5) . . . . ?
C20 C21 C22 O13 4.5(9) . . . . ?
C22 O12 C23 C24 -169.8(8) . . . . ?
C23 O12 C22 O13 1.4(9) . . . . ?
C23 O12 C22 C21 -177.5(6) . . . . ?

_olex2_date_sample_data_collection 2014-08-29
_olex2_date_sample_submission    1409266800
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id xstr0280
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
####################################################################### 
# 
# 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_str0555
_database_code_depnum_ccdc_archive 'CCDC 1509601'
_audit_update_record             
;
2016-10-12 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_audit_creation_date             2016-10-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H15 N O13 Os3 S'
_chemical_formula_sum            'C24 H15 N O13 Os3 S'
_chemical_formula_weight         1128.03
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0477(16)
_cell_length_b                   16.538(3)
_cell_length_c                   17.657(3)
_cell_angle_alpha                75.769(2)
_cell_angle_beta                 84.515(2)
_cell_angle_gamma                84.498(2)
_cell_volume                     2823.1(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5247
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.39
_shelx_estimated_absorpt_T_max   0.193
_shelx_estimated_absorpt_T_min   0.066
_exptl_absorpt_coefficient_mu    13.610
_exptl_absorpt_correction_T_max  0.1932
_exptl_absorpt_correction_T_min  0.145703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1880 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.1457.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.654
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21541
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.274
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9293
_reflns_number_total             10939
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.786
_refine_diff_density_min         -1.890
_refine_diff_density_rms         0.273
_refine_ls_extinction_coef       0.00013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         10939
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0448P)²+4.9046P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1067
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C24(H24), C74(H74)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C26(H26A,H26B), C71(H71A,H71B), C76(H76A,H76B)
2.c Me refined with riding coordinates:
 C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C70(H70A,H70B,H70C), C77(H77A,H77B,
 H77C)
2.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C14(H14), C15(H15), C60(H60), C63(H63), C64(H64), C65(H65)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.26739(3) 0.32033(2) 0.27539(2) 0.01837(9) Uani 1 1 d . . . . .
Os2 Os 0.19198(3) 0.15336(2) 0.30546(2) 0.01887(9) Uani 1 1 d . . . . .
Os3 Os -0.07268(3) 0.15964(2) 0.25064(2) 0.01818(9) Uani 1 1 d . . . . .
C1 C 0.2087(8) 0.4341(5) 0.2402(5) 0.0273(18) Uani 1 1 d . . . . .
C2 C 0.4553(10) 0.3293(6) 0.2810(5) 0.035(2) Uani 1 1 d . . . . .
C3 C 0.2301(8) 0.3222(5) 0.3855(5) 0.0278(19) Uani 1 1 d . . . . .
C4 C 0.3725(9) 0.1500(5) 0.3329(5) 0.032(2) Uani 1 1 d . . . . .
C5 C 0.1105(8) 0.1448(5) 0.4064(5) 0.0261(18) Uani 1 1 d . . . . .
C6 C 0.1743(9) 0.0375(5) 0.3181(5) 0.0311(19) Uani 1 1 d . . . . .
C7 C -0.1275(8) 0.0630(5) 0.3278(5) 0.0265(18) Uani 1 1 d . . . . .
C8 C -0.0130(8) 0.0922(5) 0.1822(5) 0.0222(16) Uani 1 1 d . . . . .
C9 C -0.2406(8) 0.1889(5) 0.2030(5) 0.0254(17) Uani 1 1 d . . . . .
O1 O 0.1691(6) 0.5022(4) 0.2192(4) 0.0340(14) Uani 1 1 d . . . . .
O2 O 0.5670(6) 0.3340(5) 0.2831(5) 0.053(2) Uani 1 1 d . . . . .
O3 O 0.2128(6) 0.3248(4) 0.4492(3) 0.0330(14) Uani 1 1 d . . . . .
O4 O 0.4807(6) 0.1367(4) 0.3532(4) 0.0426(17) Uani 1 1 d . . . . .
O5 O 0.0591(7) 0.1395(4) 0.4688(4) 0.0413(16) Uani 1 1 d . . . . .
O6 O 0.1619(7) -0.0322(4) 0.3257(4) 0.0423(16) Uani 1 1 d . . . . .
O7 O -0.1608(7) 0.0038(4) 0.3749(3) 0.0384(15) Uani 1 1 d . . . . .
O8 O 0.0250(6) 0.0497(4) 0.1403(3) 0.0305(13) Uani 1 1 d . . . . .
O9 O -0.3392(6) 0.2053(4) 0.1743(4) 0.0355(15) Uani 1 1 d . . . . .
N1 N 0.2861(6) 0.1586(4) 0.1881(4) 0.0216(14) Uani 1 1 d . . . . .
S1 S 0.3886(2) 0.11687(15) 0.06338(14) 0.0347(5) Uani 1 1 d . . . . .
O10 O -0.1312(5) 0.2424(3) 0.3267(3) 0.0208(11) Uani 1 1 d . . . . .
O11 O -0.0324(5) 0.3402(3) 0.3629(3) 0.0233(12) Uani 1 1 d . . . . .
O12 O -0.1296(6) 0.3968(3) 0.1888(3) 0.0287(13) Uani 1 1 d . . . . .
O13 O -0.1072(6) 0.3394(3) 0.0842(3) 0.0283(13) Uani 1 1 d . . . . .
C10 C 0.3125(8) 0.0955(5) 0.1553(5) 0.0261(18) Uani 1 1 d . . . . .
H10 H 0.2906 0.0417 0.1810 0.031 Uiso 1 1 calc R . . . .
C11 C 0.3313(7) 0.2332(5) 0.1382(4) 0.0191(16) Uani 1 1 d . . . . .
C12 C 0.3251(8) 0.3101(5) 0.1583(4) 0.0236(17) Uani 1 1 d . . . . .
C13 C 0.3722(8) 0.3750(5) 0.1002(5) 0.0284(19) Uani 1 1 d . . . . .
H13 H 0.3710 0.4279 0.1098 0.034 Uiso 1 1 calc R . . . .
C14 C 0.4238(8) 0.3621(6) 0.0240(5) 0.030(2) Uani 1 1 d . . . . .
H14 H 0.4505 0.4078 -0.0149 0.037 Uiso 1 1 calc R . . . .
C15 C 0.4341(8) 0.2881(6) 0.0081(5) 0.034(2) Uani 1 1 d . . . . .
H15 H 0.4724 0.2807 -0.0401 0.040 Uiso 1 1 calc R . . . .
C16 C 0.3864(7) 0.2212(5) 0.0649(5) 0.0255(18) Uani 1 1 d . . . . .
C20 C -0.1226(12) 0.4162(8) 0.4555(7) 0.064(4) Uani 1 1 d . . . . .
H20A H -0.1913 0.4205 0.4963 0.096 Uiso 1 1 calc R . . . .
H20B H -0.1278 0.4661 0.4142 0.096 Uiso 1 1 calc R . . . .
H20C H -0.0362 0.4092 0.4763 0.096 Uiso 1 1 calc R . . . .
C21 C -0.1420(10) 0.3421(6) 0.4238(5) 0.039(2) Uani 1 1 d . . . . .
H21A H -0.1373 0.2909 0.4649 0.047 Uiso 1 1 calc R . . . .
H21B H -0.2283 0.3484 0.4018 0.047 Uiso 1 1 calc R . . . .
C22 C -0.0339(8) 0.2867(5) 0.3198(4) 0.0213(17) Uani 1 1 d . . . . .
C23 C 0.0813(7) 0.2782(4) 0.2627(4) 0.0169(15) Uani 1 1 d . . . . .
C24 C 0.0184(7) 0.2733(4) 0.1879(4) 0.0170(15) Uani 1 1 d . . . . .
H24 H 0.0870 0.2626 0.1475 0.020 Uiso 1 1 calc R . . . .
C25 C -0.0787(8) 0.3432(5) 0.1561(4) 0.0245(17) Uani 1 1 d . . . . .
C26 C -0.2111(10) 0.4021(6) 0.0475(6) 0.042(2) Uani 1 1 d . . . . .
H26A H -0.2934 0.3990 0.0813 0.051 Uiso 1 1 calc R . . . .
H26B H -0.1813 0.4580 0.0382 0.051 Uiso 1 1 calc R . . . .
C27 C -0.2328(9) 0.3825(6) -0.0268(5) 0.039(2) Uani 1 1 d . . . . .
H27A H -0.3000 0.4219 -0.0529 0.059 Uiso 1 1 calc R . . . .
H27B H -0.2621 0.3270 -0.0166 0.059 Uiso 1 1 calc R . . . .
H27C H -0.1505 0.3857 -0.0595 0.059 Uiso 1 1 calc R . . . .
Os51 Os 0.27531(3) 0.17758(2) 0.70439(2) 0.01812(9) Uani 1 1 d . . . . .
Os52 Os 0.35236(3) 0.34501(2) 0.66732(2) 0.01887(9) Uani 1 1 d . . . . .
Os53 Os 0.61259(3) 0.34035(2) 0.72811(2) 0.01824(9) Uani 1 1 d . . . . .
C51 C 0.3221(9) 0.0644(5) 0.7487(5) 0.0304(19) Uani 1 1 d . . . . .
C52 C 0.0867(10) 0.1708(6) 0.6954(6) 0.036(2) Uani 1 1 d . . . . .
C53 C 0.3176(8) 0.1630(5) 0.5982(5) 0.0276(19) Uani 1 1 d . . . . .
C54 C 0.4339(8) 0.3459(5) 0.5659(5) 0.0272(19) Uani 1 1 d . . . . .
C55 C 0.1707(9) 0.3466(5) 0.6380(5) 0.032(2) Uani 1 1 d . . . . .
C56 C 0.3769(9) 0.4608(5) 0.6491(5) 0.0296(19) Uani 1 1 d . . . . .
C57 C 0.7764(8) 0.3115(5) 0.7790(5) 0.0274(18) Uani 1 1 d . . . . .
C58 C 0.5461(7) 0.4101(5) 0.7944(4) 0.0189(15) Uani 1 1 d . . . . .
C59 C 0.6768(8) 0.4354(5) 0.6506(5) 0.0271(18) Uani 1 1 d . . . . .
O51 O 0.3561(7) -0.0048(4) 0.7746(4) 0.0447(17) Uani 1 1 d . . . . .
O52 O -0.0260(7) 0.1707(5) 0.6917(5) 0.0518(19) Uani 1 1 d . . . . .
O53 O 0.3322(6) 0.1536(4) 0.5363(3) 0.0348(14) Uani 1 1 d . . . . .
O54 O 0.4863(7) 0.3474(4) 0.5054(4) 0.0402(16) Uani 1 1 d . . . . .
O55 O 0.0657(6) 0.3587(4) 0.6174(4) 0.0414(16) Uani 1 1 d . . . . .
O56 O 0.3942(7) 0.5314(4) 0.6353(4) 0.0464(18) Uani 1 1 d . . . . .
O57 O 0.8750(6) 0.2949(4) 0.8091(4) 0.0396(16) Uani 1 1 d . . . . .
O58 O 0.5067(6) 0.4525(4) 0.8348(3) 0.0299(13) Uani 1 1 d . . . . .
O59 O 0.7149(7) 0.4923(4) 0.6051(4) 0.0430(17) Uani 1 1 d . . . . .
N51 N 0.2509(6) 0.3470(4) 0.7822(4) 0.0252(15) Uani 1 1 d . . . . .
S51 S 0.1387(2) 0.39880(16) 0.89938(15) 0.0379(5) Uani 1 1 d . . . . .
O60 O 0.6750(5) 0.2555(3) 0.6554(3) 0.0235(12) Uani 1 1 d . . . . .
O61 O 0.5778(6) 0.1590(3) 0.6155(3) 0.0260(12) Uani 1 1 d . . . . .
O62 O 0.6613(6) 0.1022(4) 0.7963(3) 0.0316(14) Uani 1 1 d . . . . .
O63 O 0.6417(5) 0.1621(3) 0.8978(3) 0.0242(12) Uani 1 1 d . . . . .
C60 C 0.2217(8) 0.4151(5) 0.8094(5) 0.0267(18) Uani 1 1 d . . . . .
H60 H 0.2451 0.4678 0.7813 0.032 Uiso 1 1 calc R . . . .
C61 C 0.2047(7) 0.2754(5) 0.8345(4) 0.0209(16) Uani 1 1 d . . . . .
C62 C 0.2115(8) 0.1974(5) 0.8194(4) 0.0229(17) Uani 1 1 d . . . . .
C63 C 0.1572(8) 0.1354(6) 0.8790(5) 0.0299(19) Uani 1 1 d . . . . .
H63 H 0.1565 0.0814 0.8724 0.036 Uiso 1 1 calc R . . . .
C64 C 0.1031(8) 0.1548(6) 0.9498(4) 0.0279(19) Uani 1 1 d . . . . .
H64 H 0.0737 0.1107 0.9899 0.033 Uiso 1 1 calc R . . . .
C65 C 0.0910(8) 0.2272(6) 0.9635(5) 0.036(2) Uani 1 1 d . . . . .
H65 H 0.0508 0.2367 1.0105 0.043 Uiso 1 1 calc R . . . .
C66 C 0.1421(8) 0.2926(5) 0.9031(5) 0.0265(18) Uani 1 1 d . . . . .
C70 C 0.6717(11) 0.0943(8) 0.5141(7) 0.065(4) Uani 1 1 d . . . . .
H70A H 0.7406 0.0950 0.4725 0.098 Uiso 1 1 calc R . . . .
H70B H 0.5854 0.1011 0.4933 0.098 Uiso 1 1 calc R . . . .
H70C H 0.6801 0.0418 0.5522 0.098 Uiso 1 1 calc R . . . .
C71 C 0.6855(9) 0.1635(6) 0.5518(5) 0.038(2) Uani 1 1 d . . . . .
H71A H 0.7726 0.1575 0.5728 0.045 Uiso 1 1 calc R . . . .
H71B H 0.6768 0.2169 0.5139 0.045 Uiso 1 1 calc R . . . .
C72 C 0.5776(7) 0.2111(5) 0.6609(4) 0.0195(16) Uani 1 1 d . . . . .
C73 C 0.4607(7) 0.2200(4) 0.7166(4) 0.0166(15) Uani 1 1 d . . . . .
C74 C 0.5190(7) 0.2277(4) 0.7907(4) 0.0161(14) Uani 1 1 d . . . . .
H74 H 0.4480 0.2398 0.8294 0.019 Uiso 1 1 calc R . . . .
C75 C 0.6130(8) 0.1581(5) 0.8265(4) 0.0197(16) Uani 1 1 d . . . . .
C76 C 0.7403(10) 0.1007(6) 0.9356(5) 0.039(2) Uani 1 1 d . . . . .
H76A H 0.8240 0.1042 0.9031 0.046 Uiso 1 1 calc R . . . .
H76B H 0.7103 0.0452 0.9424 0.046 Uiso 1 1 calc R . . . .
C77 C 0.7615(9) 0.1152(6) 1.0126(5) 0.035(2) Uani 1 1 d . . . . .
H77A H 0.8285 0.0745 1.0372 0.052 Uiso 1 1 calc R . . . .
H77B H 0.6790 0.1103 1.0451 0.052 Uiso 1 1 calc R . . . .
H77C H 0.7908 0.1703 1.0056 0.052 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 Os2 2.8434(6) . ?
Os1 C1 1.885(9) . ?
Os1 C2 1.922(10) . ?
Os1 C3 1.952(9) . ?
Os1 C12 2.136(8) . ?
Os1 C23 2.107(7) . ?
Os2 Os3 2.8999(6) . ?
Os2 C4 1.914(9) . ?
Os2 C5 1.867(8) . ?
Os2 C6 1.898(9) . ?
Os2 N1 2.179(7) . ?
Os2 C23 2.241(7) . ?
Os3 C7 1.915(9) . ?
Os3 C8 1.860(8) . ?
Os3 C9 1.924(8) . ?
Os3 O10 2.151(5) . ?
Os3 C24 2.170(7) . ?
C1 O1 1.142(10) . ?
C2 O2 1.136(11) . ?
C3 O3 1.131(10) . ?
C4 O4 1.162(10) . ?
C5 O5 1.159(10) . ?
C6 O6 1.144(10) . ?
C7 O7 1.171(10) . ?
C8 O8 1.156(10) . ?
C9 O9 1.135(9) . ?
N1 C10 1.307(10) . ?
N1 C11 1.416(10) . ?
S1 C10 1.697(9) . ?
S1 C16 1.731(9) . ?
O10 C22 1.256(9) . ?
O11 C21 1.468(10) . ?
O11 C22 1.302(9) . ?
O12 C25 1.220(10) . ?
O13 C25 1.345(9) . ?
O13 C26 1.475(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.396(11) . ?
C11 C16 1.410(11) . ?
C12 C13 1.375(12) . ?
C13 H13 0.9300 . ?
C13 C14 1.453(11) . ?
C14 H14 0.9300 . ?
C14 C15 1.314(13) . ?
C15 H15 0.9300 . ?
C15 C16 1.387(12) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C20 C21 1.502(14) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.480(11) . ?
C23 C24 1.540(10) . ?
C24 H24 0.9800 . ?
C24 C25 1.474(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.467(13) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
Os51 Os52 2.8493(6) . ?
Os51 C51 1.876(8) . ?
Os51 C52 1.933(9) . ?
Os51 C53 1.950(9) . ?
Os51 C62 2.163(8) . ?
Os51 C73 2.100(7) . ?
Os52 Os53 2.9072(6) . ?
Os52 C54 1.894(9) . ?
Os52 C55 1.940(9) . ?
Os52 C56 1.899(8) . ?
Os52 N51 2.188(7) . ?
Os52 C73 2.254(6) . ?
Os53 C57 1.914(8) . ?
Os53 C58 1.875(8) . ?
Os53 C59 1.930(8) . ?
Os53 O60 2.139(5) . ?
Os53 C74 2.168(7) . ?
C51 O51 1.155(10) . ?
C52 O52 1.141(11) . ?
C53 O53 1.137(10) . ?
C54 O54 1.140(10) . ?
C55 O55 1.132(10) . ?
C56 O56 1.159(10) . ?
C57 O57 1.148(10) . ?
C58 O58 1.137(9) . ?
C59 O59 1.147(10) . ?
N51 C60 1.327(10) . ?
N51 C61 1.399(10) . ?
S51 C60 1.694(9) . ?
S51 C66 1.738(9) . ?
O60 C72 1.261(9) . ?
O61 C71 1.477(10) . ?
O61 C72 1.314(9) . ?
O62 C75 1.217(9) . ?
O63 C75 1.337(9) . ?
O63 C76 1.434(9) . ?
C60 H60 0.9300 . ?
C61 C62 1.374(11) . ?
C61 C66 1.392(11) . ?
C62 C63 1.387(11) . ?
C63 H63 0.9300 . ?
C63 C64 1.412(12) . ?
C64 H64 0.9300 . ?
C64 C65 1.272(13) . ?
C65 H65 0.9300 . ?
C65 C66 1.416(12) . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C70 C71 1.481(14) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C72 C73 1.478(10) . ?
C73 C74 1.522(10) . ?
C74 H74 0.9800 . ?
C74 C75 1.471(10) . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C76 C77 1.476(12) . ?
C77 H77A 0.9600 . ?
C77 H77B 0.9600 . ?
C77 H77C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Os1 Os2 144.7(2) . . ?
C1 Os1 C2 100.5(4) . . ?
C1 Os1 C3 93.0(3) . . ?
C1 Os1 C12 91.5(3) . . ?
C1 Os1 C23 93.5(3) . . ?
C2 Os1 Os2 114.4(3) . . ?
C2 Os1 C3 91.4(4) . . ?
C2 Os1 C12 84.5(3) . . ?
C2 Os1 C23 164.0(3) . . ?
C3 Os1 Os2 91.5(2) . . ?
C3 Os1 C12 174.4(3) . . ?
C3 Os1 C23 95.7(3) . . ?
C12 Os1 Os2 86.7(2) . . ?
C23 Os1 Os2 51.24(18) . . ?
C23 Os1 C12 87.4(3) . . ?
Os1 Os2 Os3 107.769(12) . . ?
C4 Os2 Os1 71.6(3) . . ?
C4 Os2 Os3 175.2(3) . . ?
C4 Os2 N1 83.9(3) . . ?
C4 Os2 C23 118.7(3) . . ?
C5 Os2 Os1 98.5(3) . . ?
C5 Os2 Os3 88.2(2) . . ?
C5 Os2 C4 96.5(4) . . ?
C5 Os2 C6 88.8(4) . . ?
C5 Os2 N1 177.9(3) . . ?
C5 Os2 C23 91.0(3) . . ?
C6 Os2 Os1 169.4(3) . . ?
C6 Os2 Os3 79.9(3) . . ?
C6 Os2 C4 100.1(4) . . ?
C6 Os2 N1 89.1(3) . . ?
C6 Os2 C23 140.9(3) . . ?
N1 Os2 Os1 83.55(17) . . ?
N1 Os2 Os3 91.34(16) . . ?
N1 Os2 C23 90.6(2) . . ?
C23 Os2 Os1 47.14(19) . . ?
C23 Os2 Os3 61.02(19) . . ?
C7 Os3 Os2 95.2(2) . . ?
C7 Os3 C9 96.9(3) . . ?
C7 Os3 O10 93.2(3) . . ?
C7 Os3 C24 165.0(3) . . ?
C8 Os3 Os2 92.5(2) . . ?
C8 Os3 C7 89.8(3) . . ?
C8 Os3 C9 91.5(3) . . ?
C8 Os3 O10 176.3(3) . . ?
C8 Os3 C24 98.9(3) . . ?
C9 Os3 Os2 167.3(2) . . ?
C9 Os3 O10 90.2(3) . . ?
C9 Os3 C24 95.2(3) . . ?
O10 Os3 Os2 85.13(13) . . ?
O10 Os3 C24 77.8(2) . . ?
C24 Os3 Os2 72.28(17) . . ?
O1 C1 Os1 177.8(7) . . ?
O2 C2 Os1 178.6(8) . . ?
O3 C3 Os1 177.4(8) . . ?
O4 C4 Os2 170.9(8) . . ?
O5 C5 Os2 179.5(7) . . ?
O6 C6 Os2 179.1(8) . . ?
O7 C7 Os3 179.9(9) . . ?
O8 C8 Os3 179.2(7) . . ?
O9 C9 Os3 179.0(8) . . ?
C10 N1 Os2 126.2(6) . . ?
C10 N1 C11 111.2(7) . . ?
C11 N1 Os2 122.6(5) . . ?
C10 S1 C16 89.9(4) . . ?
C22 O10 Os3 104.7(5) . . ?
C22 O11 C21 118.0(7) . . ?
C25 O13 C26 115.8(6) . . ?
N1 C10 S1 116.5(7) . . ?
N1 C10 H10 121.8 . . ?
S1 C10 H10 121.8 . . ?
C12 C11 N1 124.8(7) . . ?
C12 C11 C16 123.0(7) . . ?
C16 C11 N1 112.1(7) . . ?
C11 C12 Os1 121.1(6) . . ?
C13 C12 Os1 123.3(6) . . ?
C13 C12 C11 115.2(7) . . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 120.9(8) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 118.8 . . ?
C15 C14 C13 122.4(8) . . ?
C15 C14 H14 118.8 . . ?
C14 C15 H15 120.9 . . ?
C14 C15 C16 118.3(8) . . ?
C16 C15 H15 120.9 . . ?
C11 C16 S1 110.2(6) . . ?
C15 C16 S1 129.7(7) . . ?
C15 C16 C11 120.0(8) . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
O11 C21 C20 105.4(8) . . ?
O11 C21 H21A 110.7 . . ?
O11 C21 H21B 110.7 . . ?
C20 C21 H21A 110.7 . . ?
C20 C21 H21B 110.7 . . ?
H21A C21 H21B 108.8 . . ?
O10 C22 O11 120.7(7) . . ?
O10 C22 C23 120.2(7) . . ?
O11 C22 C23 119.1(7) . . ?
Os1 C23 Os2 81.6(2) . . ?
C22 C23 Os1 120.0(5) . . ?
C22 C23 Os2 108.2(4) . . ?
C22 C23 C24 105.0(6) . . ?
C24 C23 Os1 129.6(5) . . ?
C24 C23 Os2 105.9(4) . . ?
Os3 C24 H24 111.6 . . ?
C23 C24 Os3 90.5(4) . . ?
C23 C24 H24 111.6 . . ?
C25 C24 Os3 114.1(5) . . ?
C25 C24 C23 116.0(6) . . ?
C25 C24 H24 111.6 . . ?
O12 C25 O13 123.3(7) . . ?
O12 C25 C24 126.7(7) . . ?
O13 C25 C24 110.0(7) . . ?
O13 C26 H26A 110.4 . . ?
O13 C26 H26B 110.4 . . ?
H26A C26 H26B 108.6 . . ?
C27 C26 O13 106.5(7) . . ?
C27 C26 H26A 110.4 . . ?
C27 C26 H26B 110.4 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C51 Os51 Os52 147.0(3) . . ?
C51 Os51 C52 99.0(4) . . ?
C51 Os51 C53 92.2(4) . . ?
C51 Os51 C62 90.3(3) . . ?
C51 Os51 C73 95.6(3) . . ?
C52 Os51 Os52 113.2(3) . . ?
C52 Os51 C53 90.7(4) . . ?
C52 Os51 C62 84.8(3) . . ?
C52 Os51 C73 163.5(3) . . ?
C53 Os51 Os52 94.3(2) . . ?
C53 Os51 C62 175.2(3) . . ?
C53 Os51 C73 96.4(3) . . ?
C62 Os51 Os52 85.7(2) . . ?
C73 Os51 Os52 51.52(18) . . ?
C73 Os51 C62 87.4(3) . . ?
Os51 Os52 Os53 107.246(12) . . ?
C54 Os52 Os51 97.0(2) . . ?
C54 Os52 Os53 91.1(2) . . ?
C54 Os52 C55 94.8(4) . . ?
C54 Os52 C56 89.3(4) . . ?
C54 Os52 N51 177.6(3) . . ?
C54 Os52 C73 90.8(3) . . ?
C55 Os52 Os51 71.4(2) . . ?
C55 Os52 Os53 174.0(3) . . ?
C55 Os52 N51 83.1(3) . . ?
C55 Os52 C73 118.2(3) . . ?
C56 Os52 Os51 171.2(3) . . ?
C56 Os52 Os53 78.6(2) . . ?
C56 Os52 C55 102.1(3) . . ?
C56 Os52 N51 89.9(3) . . ?
C56 Os52 C73 139.6(3) . . ?
N51 Os52 Os51 83.52(18) . . ?
N51 Os52 Os53 90.92(16) . . ?
N51 Os52 C73 91.2(3) . . ?
C73 Os52 Os51 46.83(19) . . ?
C73 Os52 Os53 60.97(19) . . ?
C57 Os53 Os52 167.0(3) . . ?
C57 Os53 C59 95.4(4) . . ?
C57 Os53 O60 90.1(3) . . ?
C57 Os53 C74 95.0(3) . . ?
C58 Os53 Os52 92.3(2) . . ?
C58 Os53 C57 92.3(3) . . ?
C58 Os53 C59 90.4(3) . . ?
C58 Os53 O60 175.6(3) . . ?
C58 Os53 C74 98.6(3) . . ?
C59 Os53 Os52 96.7(2) . . ?
C59 Os53 O60 93.1(3) . . ?
C59 Os53 C74 165.9(3) . . ?
O60 Os53 Os52 84.56(14) . . ?
O60 Os53 C74 77.5(2) . . ?
C74 Os53 Os52 72.25(17) . . ?
O51 C51 Os51 177.2(8) . . ?
O52 C52 Os51 176.2(8) . . ?
O53 C53 Os51 174.8(7) . . ?
O54 C54 Os52 177.9(8) . . ?
O55 C55 Os52 170.8(8) . . ?
O56 C56 Os52 177.4(9) . . ?
O57 C57 Os53 179.3(8) . . ?
O58 C58 Os53 179.5(7) . . ?
O59 C59 Os53 179.4(7) . . ?
C60 N51 Os52 124.9(6) . . ?
C60 N51 C61 112.3(7) . . ?
C61 N51 Os52 122.8(5) . . ?
C60 S51 C66 90.0(4) . . ?
C72 O60 Os53 105.0(5) . . ?
C72 O61 C71 117.4(6) . . ?
C75 O63 C76 117.0(6) . . ?
N51 C60 S51 114.9(7) . . ?
N51 C60 H60 122.5 . . ?
S51 C60 H60 122.5 . . ?
C62 C61 N51 125.1(7) . . ?
C62 C61 C66 122.7(8) . . ?
C66 C61 N51 112.1(7) . . ?
C61 C62 Os51 121.7(6) . . ?
C61 C62 C63 115.5(8) . . ?
C63 C62 Os51 122.2(6) . . ?
C62 C63 H63 120.2 . . ?
C62 C63 C64 119.7(8) . . ?
C64 C63 H63 120.2 . . ?
C63 C64 H64 117.2 . . ?
C65 C64 C63 125.6(8) . . ?
C65 C64 H64 117.2 . . ?
C64 C65 H65 121.9 . . ?
C64 C65 C66 116.3(8) . . ?
C66 C65 H65 121.9 . . ?
C61 C66 S51 110.7(6) . . ?
C61 C66 C65 120.1(8) . . ?
C65 C66 S51 129.3(7) . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C71 C70 H70A 109.5 . . ?
C71 C70 H70B 109.5 . . ?
C71 C70 H70C 109.5 . . ?
O61 C71 C70 107.1(8) . . ?
O61 C71 H71A 110.3 . . ?
O61 C71 H71B 110.3 . . ?
C70 C71 H71A 110.3 . . ?
C70 C71 H71B 110.3 . . ?
H71A C71 H71B 108.5 . . ?
O60 C72 O61 120.1(7) . . ?
O60 C72 C73 120.0(7) . . ?
O61 C72 C73 119.9(7) . . ?
Os51 C73 Os52 81.7(2) . . ?
C72 C73 Os51 121.0(5) . . ?
C72 C73 Os52 106.4(4) . . ?
C72 C73 C74 105.4(6) . . ?
C74 C73 Os51 128.8(5) . . ?
C74 C73 Os52 106.2(4) . . ?
Os53 C74 H74 111.2 . . ?
C73 C74 Os53 91.4(4) . . ?
C73 C74 H74 111.2 . . ?
C75 C74 Os53 114.6(5) . . ?
C75 C74 C73 116.0(6) . . ?
C75 C74 H74 111.2 . . ?
O62 C75 O63 122.2(7) . . ?
O62 C75 C74 125.4(7) . . ?
O63 C75 C74 112.4(6) . . ?
O63 C76 H76A 109.7 . . ?
O63 C76 H76B 109.7 . . ?
O63 C76 C77 109.9(7) . . ?
H76A C76 H76B 108.2 . . ?
C77 C76 H76A 109.7 . . ?
C77 C76 H76B 109.7 . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Os1 C12 C13 C14 173.2(6) . . . . ?
Os1 C23 C24 Os3 145.0(5) . . . . ?
Os1 C23 C24 C25 -97.7(8) . . . . ?
Os2 N1 C10 S1 -179.2(3) . . . . ?
Os2 N1 C11 C12 2.0(9) . . . . ?
Os2 N1 C11 C16 -178.9(5) . . . . ?
Os2 C23 C24 Os3 52.8(4) . . . . ?
Os2 C23 C24 C25 170.1(5) . . . . ?
Os3 O10 C22 O11 -175.0(5) . . . . ?
Os3 O10 C22 C23 4.5(7) . . . . ?
Os3 C24 C25 O12 90.9(9) . . . . ?
Os3 C24 C25 O13 -88.0(7) . . . . ?
N1 C11 C12 Os1 8.1(10) . . . . ?
N1 C11 C12 C13 -178.7(7) . . . . ?
N1 C11 C16 S1 -3.5(8) . . . . ?
N1 C11 C16 C15 179.1(7) . . . . ?
O10 C22 C23 Os1 -159.9(5) . . . . ?
O10 C22 C23 Os2 -69.2(7) . . . . ?
O10 C22 C23 C24 43.5(8) . . . . ?
O11 C22 C23 Os1 19.6(8) . . . . ?
O11 C22 C23 Os2 110.3(6) . . . . ?
O11 C22 C23 C24 -137.0(6) . . . . ?
C10 N1 C11 C12 -176.0(7) . . . . ?
C10 N1 C11 C16 3.1(9) . . . . ?
C10 S1 C16 C11 2.4(6) . . . . ?
C10 S1 C16 C15 179.4(8) . . . . ?
C11 N1 C10 S1 -1.3(8) . . . . ?
C11 C12 C13 C14 0.1(11) . . . . ?
C12 C11 C16 S1 175.6(6) . . . . ?
C12 C11 C16 C15 -1.8(11) . . . . ?
C12 C13 C14 C15 -3.4(13) . . . . ?
C13 C14 C15 C16 3.9(13) . . . . ?
C14 C15 C16 S1 -178.2(7) . . . . ?
C14 C15 C16 C11 -1.4(12) . . . . ?
C16 S1 C10 N1 -0.7(6) . . . . ?
C16 C11 C12 Os1 -170.9(6) . . . . ?
C16 C11 C12 C13 2.3(11) . . . . ?
C21 O11 C22 O10 4.9(10) . . . . ?
C21 O11 C22 C23 -174.6(6) . . . . ?
C22 O11 C21 C20 -172.8(7) . . . . ?
C22 C23 C24 Os3 -61.6(5) . . . . ?
C22 C23 C24 C25 55.7(8) . . . . ?
C23 C24 C25 O12 -12.3(12) . . . . ?
C23 C24 C25 O13 168.8(6) . . . . ?
C25 O13 C26 C27 -175.8(7) . . . . ?
C26 O13 C25 O12 -3.3(12) . . . . ?
C26 O13 C25 C24 175.6(7) . . . . ?
Os51 C62 C63 C64 -172.6(6) . . . . ?
Os51 C73 C74 Os53 -144.2(4) . . . . ?
Os51 C73 C74 C75 97.3(7) . . . . ?
Os52 N51 C60 S51 178.3(3) . . . . ?
Os52 N51 C61 C62 -3.0(10) . . . . ?
Os52 N51 C61 C66 -179.2(5) . . . . ?
Os52 C73 C74 Os53 -52.0(4) . . . . ?
Os52 C73 C74 C75 -170.4(5) . . . . ?
Os53 O60 C72 O61 171.8(5) . . . . ?
Os53 O60 C72 C73 -5.9(7) . . . . ?
Os53 C74 C75 O62 -93.7(9) . . . . ?
Os53 C74 C75 O63 86.2(7) . . . . ?
N51 C61 C62 Os51 -7.5(10) . . . . ?
N51 C61 C62 C63 -178.8(7) . . . . ?
N51 C61 C66 S51 1.6(8) . . . . ?
N51 C61 C66 C65 -178.9(7) . . . . ?
O60 C72 C73 Os51 160.8(5) . . . . ?
O60 C72 C73 Os52 70.8(7) . . . . ?
O60 C72 C73 C74 -41.7(8) . . . . ?
O61 C72 C73 Os51 -16.9(9) . . . . ?
O61 C72 C73 Os52 -106.9(6) . . . . ?
O61 C72 C73 C74 140.6(6) . . . . ?
C60 N51 C61 C62 174.8(7) . . . . ?
C60 N51 C61 C66 -1.4(9) . . . . ?
C60 S51 C66 C61 -1.1(6) . . . . ?
C60 S51 C66 C65 179.5(8) . . . . ?
C61 N51 C60 S51 0.5(8) . . . . ?
C61 C62 C63 C64 -1.5(11) . . . . ?
C62 C61 C66 S51 -174.7(6) . . . . ?
C62 C61 C66 C65 4.8(12) . . . . ?
C62 C63 C64 C65 4.7(13) . . . . ?
C63 C64 C65 C66 -2.9(13) . . . . ?
C64 C65 C66 S51 177.6(7) . . . . ?
C64 C65 C66 C61 -1.7(12) . . . . ?
C66 S51 C60 N51 0.3(6) . . . . ?
C66 C61 C62 Os51 168.2(6) . . . . ?
C66 C61 C62 C63 -3.0(11) . . . . ?
C71 O61 C72 O60 -8.2(10) . . . . ?
C71 O61 C72 C73 169.5(6) . . . . ?
C72 O61 C71 C70 174.8(7) . . . . ?
C72 C73 C74 Os53 60.7(5) . . . . ?
C72 C73 C74 C75 -57.7(8) . . . . ?
C73 C74 C75 O62 10.9(11) . . . . ?
C73 C74 C75 O63 -169.2(6) . . . . ?
C75 O63 C76 C77 178.9(7) . . . . ?
C76 O63 C75 O62 4.4(11) . . . . ?
C76 O63 C75 C74 -175.5(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_exp_682
_database_code_depnum_ccdc_archive 'CCDC 1509603'
_audit_update_record             
;
2016-10-12 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_audit_creation_date             2016-10-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C25 H17 N O13 Os3 S'
_chemical_formula_sum            'C25 H17 N O13 Os3 S'
_chemical_formula_weight         1142.06
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8419(3)
_cell_length_b                   9.9715(3)
_cell_length_c                   17.3201(5)
_cell_angle_alpha                75.059(3)
_cell_angle_beta                 80.399(2)
_cell_angle_gamma                63.273(3)
_cell_volume                     1464.30(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12501
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      29.2810
_cell_measurement_theta_min      3.2720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.122
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.590
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21486
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.853
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -15.00   87.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655   77.0000    0.0000 102

#__ type_ start__ end____ width___ exp.time_
  2 omega  -17.00   82.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655   57.0000 -120.0000 99

#__ type_ start__ end____ width___ exp.time_
  3 omega  -18.00   52.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655  -99.0000 -150.0000 70

#__ type_ start__ end____ width___ exp.time_
  4 omega  -19.00   52.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655  -99.0000  -30.0000 71

#__ type_ start__ end____ width___ exp.time_
  5 omega   -4.00   63.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655 -118.0000   68.0264 67

#__ type_ start__ end____ width___ exp.time_
  6 omega  -13.00   84.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655   38.0000  150.0000 97

#__ type_ start__ end____ width___ exp.time_
  7 omega  -56.00   39.00   1.0000    1.5400
omega____ theta____ kappa____ phi______ frames
    -       11.1655  -57.0000   90.0000 95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0358578000
_diffrn_orient_matrix_UB_12      0.0398184000
_diffrn_orient_matrix_UB_13      -0.0366128000
_diffrn_orient_matrix_UB_21      0.0707039000
_diffrn_orient_matrix_UB_22      -0.0335085000
_diffrn_orient_matrix_UB_23      -0.0214983000
_diffrn_orient_matrix_UB_31      -0.0157696000
_diffrn_orient_matrix_UB_32      -0.0626109000
_diffrn_orient_matrix_UB_33      -0.0003172000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5199
_reflns_number_total             5737
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.180
_refine_diff_density_min         -2.407
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         5737
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0344P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0808
_refine_special_details          
'One Me of an a -OEt group is disordered and has been refined over two sites with 50:50 occupancy.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C17A) = Uanis(C17B)
3. Others
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=1-FVAR(1)
 Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=FVAR(1)
 Fixed Sof: H16A(0.5) H16B(0.5) H16C(0.5) H16D(0.5)
4.a Ternary CH refined with riding coordinates:
 C14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C16(H16A,H16B), C16(H16C,H16D)
4.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C21(H21)
4.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C25(H25A,H25B,H25C), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.08051(3) 0.55590(3) 0.28200(2) 0.01812(9) Uani 1 1 d . . . . .
Os2 Os 0.01197(3) 0.83123(3) 0.33144(2) 0.01802(9) Uani 1 1 d . . . . .
Os3 Os 0.26736(3) 0.91153(3) 0.27202(2) 0.01991(9) Uani 1 1 d . . . . .
S1 S -0.2340(2) 1.1354(2) 0.09193(12) 0.0340(5) Uani 1 1 d . . . . .
O1 O 0.3304(7) 0.2980(6) 0.2103(3) 0.0393(14) Uani 1 1 d . . . . .
O2 O 0.1471(6) 0.3707(6) 0.4548(3) 0.0335(13) Uani 1 1 d . . . . .
O3 O -0.1941(7) 0.4837(8) 0.2863(4) 0.0538(17) Uani 1 1 d . . . . .
O4 O -0.2805(7) 0.7811(8) 0.3752(3) 0.0485(17) Uani 1 1 d . . . . .
O5 O -0.0969(8) 1.1108(7) 0.4050(4) 0.060(2) Uani 1 1 d . . . . .
O6 O 0.1564(7) 0.6645(6) 0.4905(3) 0.0349(13) Uani 1 1 d . . . . .
O7 O 0.0749(6) 1.2108(6) 0.1676(3) 0.0330(12) Uani 1 1 d . . . . .
O8 O 0.2422(10) 1.0737(7) 0.4067(4) 0.066(2) Uani 1 1 d . . . . .
O9 O 0.5595(8) 0.9328(7) 0.1945(4) 0.0569(18) Uani 1 1 d . . . . .
O10 O 0.4048(5) 0.6869(5) 0.3371(3) 0.0217(10) Uani 1 1 d . . . . .
O11 O 0.4026(5) 0.4574(5) 0.3597(3) 0.0214(10) Uani 1 1 d . . . . .
O12 O 0.5149(6) 0.5607(6) 0.1887(3) 0.0352(13) Uani 1 1 d . . . . .
O13 O 0.4366(5) 0.7636(5) 0.0866(3) 0.0278(11) Uani 1 1 d . . . . .
N1 N -0.0911(6) 0.9417(6) 0.2137(4) 0.0252(14) Uani 1 1 d . . . . .
C1 C 0.2321(9) 0.3951(9) 0.2364(4) 0.0280(17) Uani 1 1 d . . . . .
C2 C 0.1271(8) 0.4391(8) 0.3906(4) 0.0233(16) Uani 1 1 d . . . . .
C3 C -0.0943(9) 0.5097(9) 0.2867(4) 0.0307(18) Uani 1 1 d . . . . .
C4 C -0.1660(10) 0.7867(9) 0.3573(4) 0.0345(19) Uani 1 1 d . . . . .
C5 C -0.0610(9) 1.0126(9) 0.3729(5) 0.0345(19) Uani 1 1 d . . . . .
C6 C 0.1023(9) 0.7271(8) 0.4306(4) 0.0245(16) Uani 1 1 d . . . . .
C7 C 0.1459(8) 1.0979(8) 0.2082(4) 0.0256(16) Uani 1 1 d . . . . .
C8 C 0.2517(10) 1.0118(9) 0.3585(5) 0.037(2) Uani 1 1 d . . . . .
C9 C 0.4522(10) 0.9245(9) 0.2232(5) 0.038(2) Uani 1 1 d . . . . .
C10 C 0.5378(12) 0.2506(13) 0.4623(6) 0.072(4) Uani 1 1 d . . . . .
H10A H 0.5274 0.1889 0.4298 0.109 Uiso 1 1 calc GR . . . .
H10B H 0.4546 0.2724 0.5039 0.109 Uiso 1 1 calc GR . . . .
H10C H 0.6357 0.1938 0.4875 0.109 Uiso 1 1 calc GR . . . .
C11 C 0.5314(9) 0.3963(9) 0.4108(5) 0.0335(18) Uani 1 1 d . . . . .
H11A H 0.5160 0.4699 0.4439 0.040 Uiso 1 1 calc R . . . .
H11B H 0.6276 0.3782 0.3775 0.040 Uiso 1 1 calc R . . . .
C12 C 0.3513(7) 0.6024(7) 0.3254(4) 0.0163(13) Uani 1 1 d . . . . .
C13 C 0.2222(7) 0.6675(6) 0.2716(3) 0.0124(13) Uani 1 1 d . . . . .
C14 C 0.2664(7) 0.7665(7) 0.1977(4) 0.0134(13) Uiso 1 1 d . . . . .
H14 H 0.1844 0.8226 0.1587 0.016 Uiso 1 1 calc R . . . .
C15 C 0.4154(8) 0.6839(8) 0.1594(4) 0.0220(15) Uani 1 1 d . . . . .
C18 C 0.0047(8) 0.6971(8) 0.1676(4) 0.0245(16) Uani 1 1 d . . . . .
C19 C 0.0145(9) 0.6350(10) 0.1015(4) 0.0345(19) Uani 1 1 d . . . . .
H19 H 0.0630 0.5266 0.1069 0.041 Uiso 1 1 calc R . . . .
C20 C -0.0447(10) 0.7269(11) 0.0281(5) 0.043(2) Uani 1 1 d . . . . .
H20 H -0.0312 0.6810 -0.0160 0.052 Uiso 1 1 calc R . . . .
C21 C -0.1230(8) 0.8850(8) 0.0197(4) 0.0232(16) Uani 1 1 d . . . . .
H21 H -0.1670 0.9487 -0.0290 0.028 Uiso 1 1 calc R . . . .
C22 C -0.1345(8) 0.9457(8) 0.0839(4) 0.0270(16) Uani 1 1 d . . . . .
C23 C -0.0691(8) 0.8550(9) 0.1564(4) 0.0242(16) Uani 1 1 d . . . . .
C24 C -0.1814(8) 1.0866(8) 0.1889(5) 0.0294(17) Uani 1 1 d . . . . .
C25 C -0.2507(10) 1.2098(9) 0.2349(6) 0.046(2) Uani 1 1 d . . . . .
H25A H -0.3211 1.3040 0.2018 0.069 Uiso 1 1 calc GR . . . .
H25B H -0.1704 1.2286 0.2505 0.069 Uiso 1 1 calc GR . . . .
H25C H -0.3065 1.1788 0.2831 0.069 Uiso 1 1 calc GR . . . .
C16 C 0.5896(10) 0.6963(12) 0.0456(6) 0.056(3) Uani 1 1 d . . . . .
H16A H 0.6689 0.6766 0.0809 0.067 Uiso 0.5 1 calc R . P A 1
H16B H 0.6077 0.5974 0.0339 0.067 Uiso 0.5 1 calc R . P A 1
H16C H 0.6076 0.7781 0.0052 0.067 Uiso 0.5 1 calc R . P B 2
H16D H 0.6686 0.6512 0.0851 0.067 Uiso 0.5 1 calc R . P B 2
C17A C 0.599(2) 0.801(2) -0.0279(10) 0.060(4) Uani 0.540(13) 1 d . . P C 1
H17A H 0.5227 0.8171 -0.0634 0.091 Uiso 0.540(13) 1 calc GR . P C 1
H17B H 0.7009 0.7570 -0.0542 0.091 Uiso 0.540(13) 1 calc GR . P C 1
H17C H 0.5797 0.8989 -0.0161 0.091 Uiso 0.540(13) 1 calc GR . P C 1
C17B C 0.602(2) 0.576(3) 0.0058(12) 0.060(4) Uani 0.460(13) 1 d . . P C 2
H17D H 0.5794 0.4976 0.0454 0.091 Uiso 0.460(13) 1 calc GR . P C 2
H17E H 0.7055 0.5289 -0.0180 0.091 Uiso 0.460(13) 1 calc GR . P C 2
H17F H 0.5289 0.6224 -0.0361 0.091 Uiso 0.460(13) 1 calc GR . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 Os2 2.8425(4) . ?
Os1 C1 1.878(8) . ?
Os1 C2 1.945(7) . ?
Os1 C3 1.956(7) . ?
Os1 C13 2.103(6) . ?
Os1 C18 2.139(7) . ?
Os2 Os3 2.9225(4) . ?
Os2 N1 2.220(6) . ?
Os2 C4 1.950(9) . ?
Os2 C5 1.906(8) . ?
Os2 C6 1.891(8) . ?
Os2 C13 2.267(6) . ?
Os3 O10 2.145(4) . ?
Os3 C7 1.867(8) . ?
Os3 C8 1.955(8) . ?
Os3 C9 1.919(9) . ?
Os3 C14 2.174(6) . ?
S1 C22 1.726(8) . ?
S1 C24 1.722(8) . ?
O1 C1 1.147(9) . ?
O2 C2 1.140(8) . ?
O3 C3 1.124(9) . ?
O4 C4 1.141(9) . ?
O5 C5 1.138(9) . ?
O6 C6 1.141(8) . ?
O7 C7 1.140(9) . ?
O8 C8 1.129(9) . ?
O9 C9 1.119(10) . ?
O10 C12 1.245(7) . ?
O11 C11 1.470(8) . ?
O11 C12 1.303(7) . ?
O12 C15 1.219(8) . ?
O13 C15 1.345(8) . ?
O13 C16 1.485(9) . ?
N1 C23 1.409(9) . ?
N1 C24 1.309(9) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 C11 1.476(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.498(9) . ?
C13 C14 1.533(8) . ?
C14 H14 1.0000 . ?
C14 C15 1.463(9) . ?
C18 C19 1.407(10) . ?
C18 C23 1.380(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.401(11) . ?
C20 H20 0.9500 . ?
C20 C21 1.388(12) . ?
C21 H21 0.9500 . ?
C21 C22 1.364(10) . ?
C22 C23 1.402(9) . ?
C24 C25 1.477(11) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 H16C 0.9900 . ?
C16 H16D 0.9900 . ?
C16 C17A 1.441(19) . ?
C16 C17B 1.48(2) . ?
C17A H17A 0.9800 . ?
C17A H17B 0.9800 . ?
C17A H17C 0.9800 . ?
C17B H17D 0.9800 . ?
C17B H17E 0.9800 . ?
C17B H17F 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
C1 Os1 Os2 144.9(2) . . ?
C1 Os1 C2 92.8(3) . . ?
C1 Os1 C3 100.3(3) . . ?
C1 Os1 C13 92.9(3) . . ?
C1 Os1 C18 92.6(3) . . ?
C2 Os1 Os2 90.48(19) . . ?
C2 Os1 C3 91.2(3) . . ?
C2 Os1 C13 96.7(2) . . ?
C2 Os1 C18 173.8(3) . . ?
C3 Os1 Os2 114.6(2) . . ?
C3 Os1 C13 164.3(3) . . ?
C3 Os1 C18 85.0(3) . . ?
C13 Os1 Os2 51.98(16) . . ?
C13 Os1 C18 85.9(2) . . ?
C18 Os1 Os2 86.71(19) . . ?
Os1 Os2 Os3 106.830(11) . . ?
N1 Os2 Os1 83.26(15) . . ?
N1 Os2 Os3 90.74(15) . . ?
N1 Os2 C13 89.8(2) . . ?
C4 Os2 Os1 71.4(2) . . ?
C4 Os2 Os3 172.8(2) . . ?
C4 Os2 N1 82.2(3) . . ?
C4 Os2 C13 118.4(3) . . ?
C5 Os2 Os1 171.2(3) . . ?
C5 Os2 Os3 81.9(3) . . ?
C5 Os2 N1 97.5(3) . . ?
C5 Os2 C4 99.9(4) . . ?
C5 Os2 C13 141.6(3) . . ?
C6 Os2 Os1 93.75(19) . . ?
C6 Os2 Os3 90.2(2) . . ?
C6 Os2 N1 177.0(2) . . ?
C6 Os2 C4 96.8(3) . . ?
C6 Os2 C5 85.5(3) . . ?
C6 Os2 C13 88.3(3) . . ?
C13 Os2 Os1 46.97(15) . . ?
C13 Os2 Os3 60.23(15) . . ?
O10 Os3 Os2 85.14(12) . . ?
O10 Os3 C14 78.4(2) . . ?
C7 Os3 Os2 93.3(2) . . ?
C7 Os3 O10 174.5(2) . . ?
C7 Os3 C8 91.8(3) . . ?
C7 Os3 C9 92.5(3) . . ?
C7 Os3 C14 96.1(3) . . ?
C8 Os3 Os2 96.5(3) . . ?
C8 Os3 O10 93.6(2) . . ?
C8 Os3 C14 166.7(3) . . ?
C9 Os3 Os2 167.3(2) . . ?
C9 Os3 O10 88.0(3) . . ?
C9 Os3 C8 94.6(4) . . ?
C9 Os3 C14 95.7(3) . . ?
C14 Os3 Os2 72.44(16) . . ?
C24 S1 C22 90.0(3) . . ?
C12 O10 Os3 105.0(4) . . ?
C12 O11 C11 116.7(5) . . ?
C15 O13 C16 116.3(6) . . ?
C23 N1 Os2 121.2(4) . . ?
C24 N1 Os2 127.4(5) . . ?
C24 N1 C23 111.3(6) . . ?
O1 C1 Os1 176.3(6) . . ?
O2 C2 Os1 176.4(6) . . ?
O3 C3 Os1 177.4(7) . . ?
O4 C4 Os2 170.1(8) . . ?
O5 C5 Os2 172.6(7) . . ?
O6 C6 Os2 179.8(9) . . ?
O7 C7 Os3 178.1(7) . . ?
O8 C8 Os3 177.9(7) . . ?
O9 C9 Os3 179.6(9) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
O11 C11 C10 107.1(7) . . ?
O11 C11 H11A 110.3 . . ?
O11 C11 H11B 110.3 . . ?
C10 C11 H11A 110.3 . . ?
C10 C11 H11B 110.3 . . ?
H11A C11 H11B 108.6 . . ?
O10 C12 O11 122.0(6) . . ?
O10 C12 C13 120.0(5) . . ?
O11 C12 C13 118.0(5) . . ?
Os1 C13 Os2 81.0(2) . . ?
C12 C13 Os1 120.2(4) . . ?
C12 C13 Os2 108.4(4) . . ?
C12 C13 C14 105.1(5) . . ?
C14 C13 Os1 129.4(4) . . ?
C14 C13 Os2 106.2(4) . . ?
Os3 C14 H14 112.4 . . ?
C13 C14 Os3 90.2(3) . . ?
C13 C14 H14 112.4 . . ?
C15 C14 Os3 113.9(4) . . ?
C15 C14 C13 113.8(5) . . ?
C15 C14 H14 112.4 . . ?
O12 C15 O13 121.7(6) . . ?
O12 C15 C14 126.4(6) . . ?
O13 C15 C14 111.9(6) . . ?
C19 C18 Os1 122.2(6) . . ?
C23 C18 Os1 121.6(5) . . ?
C23 C18 C19 116.0(7) . . ?
C18 C19 H19 118.8 . . ?
C20 C19 C18 122.5(8) . . ?
C20 C19 H19 118.8 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 C19 120.0(7) . . ?
C21 C20 H20 120.0 . . ?
C20 C21 H21 121.2 . . ?
C22 C21 C20 117.7(6) . . ?
C22 C21 H21 121.2 . . ?
C21 C22 S1 127.3(5) . . ?
C21 C22 C23 122.5(7) . . ?
C23 C22 S1 110.1(6) . . ?
C18 C23 N1 125.8(6) . . ?
C18 C23 C22 121.2(7) . . ?
C22 C23 N1 113.0(7) . . ?
N1 C24 S1 115.2(6) . . ?
N1 C24 C25 128.2(7) . . ?
C25 C24 S1 116.4(6) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O13 C16 H16A 109.7 . . ?
O13 C16 H16B 109.7 . . ?
O13 C16 H16C 109.5 . . ?
O13 C16 H16D 109.5 . . ?
H16A C16 H16B 108.2 . . ?
H16C C16 H16D 108.1 . . ?
C17A C16 O13 109.7(10) . . ?
C17A C16 H16A 109.7 . . ?
C17A C16 H16B 109.7 . . ?
C17B C16 O13 110.7(11) . . ?
C17B C16 H16C 109.5 . . ?
C17B C16 H16D 109.5 . . ?
C16 C17A H17A 109.5 . . ?
C16 C17A H17B 109.5 . . ?
C16 C17A H17C 109.5 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
C16 C17B H17D 109.5 . . ?
C16 C17B H17E 109.5 . . ?
C16 C17B H17F 109.5 . . ?
H17D C17B H17E 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Os1 C13 C14 Os3 145.0(4) . . . . ?
Os1 C13 C14 C15 -98.7(6) . . . . ?
Os1 C18 C19 C20 175.4(6) . . . . ?
Os1 C18 C23 N1 6.1(9) . . . . ?
Os1 C18 C23 C22 -172.3(5) . . . . ?
Os2 N1 C23 C18 5.4(9) . . . . ?
Os2 N1 C23 C22 -176.1(4) . . . . ?
Os2 N1 C24 S1 177.1(3) . . . . ?
Os2 N1 C24 C25 -7.0(11) . . . . ?
Os2 C13 C14 Os3 53.3(3) . . . . ?
Os2 C13 C14 C15 169.7(4) . . . . ?
Os3 O10 C12 O11 -176.5(5) . . . . ?
Os3 O10 C12 C13 2.5(6) . . . . ?
Os3 C14 C15 O12 85.8(7) . . . . ?
Os3 C14 C15 O13 -91.3(6) . . . . ?
S1 C22 C23 N1 -4.5(7) . . . . ?
S1 C22 C23 C18 174.1(5) . . . . ?
O10 C12 C13 Os1 -158.1(5) . . . . ?
O10 C12 C13 Os2 -67.9(6) . . . . ?
O10 C12 C13 C14 45.3(7) . . . . ?
O11 C12 C13 Os1 20.9(7) . . . . ?
O11 C12 C13 Os2 111.1(5) . . . . ?
O11 C12 C13 C14 -135.6(5) . . . . ?
C11 O11 C12 O10 -2.2(9) . . . . ?
C11 O11 C12 C13 178.8(6) . . . . ?
C12 O11 C11 C10 162.1(7) . . . . ?
C12 C13 C14 Os3 -61.4(4) . . . . ?
C12 C13 C14 C15 55.0(6) . . . . ?
C13 C14 C15 O12 -15.7(9) . . . . ?
C13 C14 C15 O13 167.2(5) . . . . ?
C15 O13 C16 C17A -174.9(11) . . . . ?
C15 O13 C16 C17B 81.7(12) . . . . ?
C18 C19 C20 C21 -3.3(13) . . . . ?
C19 C18 C23 N1 -179.4(6) . . . . ?
C19 C18 C23 C22 2.2(10) . . . . ?
C19 C20 C21 C22 2.3(12) . . . . ?
C20 C21 C22 S1 -175.9(6) . . . . ?
C20 C21 C22 C23 0.8(11) . . . . ?
C21 C22 C23 N1 178.3(6) . . . . ?
C21 C22 C23 C18 -3.2(11) . . . . ?
C22 S1 C24 N1 2.7(6) . . . . ?
C22 S1 C24 C25 -173.7(7) . . . . ?
C23 N1 C24 S1 -5.7(8) . . . . ?
C23 N1 C24 C25 170.2(8) . . . . ?
C23 C18 C19 C20 1.0(11) . . . . ?
C24 S1 C22 C21 178.2(7) . . . . ?
C24 S1 C22 C23 1.2(5) . . . . ?
C24 N1 C23 C18 -172.0(7) . . . . ?
C24 N1 C23 C22 6.5(8) . . . . ?
C16 O13 C15 O12 -2.5(10) . . . . ?
C16 O13 C15 C14 174.7(7) . . . . ?

_olex2_date_sample_data_collection 2014-10-27
_olex2_date_sample_submission    1414368000
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id xstr0308
_olex2_submission_special_instructions 'No special instructions were received'
