# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_jk112017_0m
_audit_block_doi                 10.5517/ccdc.csd.cc1z50rx
_database_code_depnum_ccdc_archive 'CCDC 1822079'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8CC01532E 2018
_audit_update_record             
;
2018-02-03 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;
_audit_creation_date             2017-11-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H4 O19 Os6'
_chemical_formula_sum            'C22 H4 O19 Os6'
_chemical_formula_weight         1713.45
_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'
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'

_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                   9.7044(5)
_cell_length_b                   11.2944(5)
_cell_length_c                   15.7359(7)
_cell_angle_alpha                82.9237(16)
_cell_angle_beta                 86.2639(16)
_cell_angle_gamma                67.6042(15)
_cell_volume                     1582.19(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.405
_cell_measurement_theta_min      4.938
_shelx_estimated_absorpt_T_max   0.326
_shelx_estimated_absorpt_T_min   0.098
_exptl_absorpt_coefficient_mu    24.077
_exptl_absorpt_correction_T_max  0.1515
_exptl_absorpt_correction_T_min  0.0615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2016'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.597
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45497
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.750
_diffrn_reflns_theta_min         2.237
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX3 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'PHOTON-100 CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6142
_reflns_number_total             7429
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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         2.337
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.289
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7429
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0294
_refine_ls_restrained_S_all      1.067
_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)+(0.0078P)²+16.0471P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0506
_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement.  R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.
;
_olex2_refinement_description    
;
1. Restrained distances
 H4-Os4
 1.8 with sigma of 0.02
 H4-Os5
 1.8 with sigma of 0.02
 H5-Os6
 1.8 with sigma of 0.02
 H5-Os4
 1.8 with sigma of 0.02
 H2-Os2
 1.8 with sigma of 0.02
 H2-Os3
 1.8 with sigma of 0.02
 H1-Os1
 1.8 with sigma of 0.02
 H1-Os2
 1.8 with sigma of 0.02
2.a Everything fixed:
 H2, H1
;
_atom_sites_solution_hydrogens   difmap
_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 0.04267(3) 0.69265(3) 0.11506(2) 0.01478(6) Uani 1 1 d D . . . .
Os2 Os 0.34375(3) 0.68891(3) 0.16723(2) 0.01457(6) Uani 1 1 d D . . . .
Os3 Os 0.10831(3) 0.68815(3) 0.28496(2) 0.01608(7) Uani 1 1 d D . . . .
Os4 Os 0.53295(3) 0.27584(3) 0.35790(2) 0.01954(7) Uani 1 1 d D . . . .
Os5 Os 0.29927(4) 0.16158(3) 0.33391(2) 0.02387(8) Uani 1 1 d D . . . .
Os6 Os 0.47470(3) 0.20942(3) 0.19884(2) 0.01553(6) Uani 1 1 d D . . . .
O5 O 0.1377(5) 0.4185(5) 0.2171(3) 0.0185(11) Uani 1 1 d . . . . .
O10 O -0.1217(6) 0.9846(5) 0.0661(4) 0.0332(14) Uani 1 1 d . . . . .
O11 O -0.2409(6) 0.6429(5) 0.1565(3) 0.0249(12) Uani 1 1 d . . . . .
O12 O 0.0690(6) 0.5944(5) -0.0603(3) 0.0262(12) Uani 1 1 d . . . . .
O20 O 0.3410(7) 0.9490(6) 0.0806(4) 0.0367(15) Uani 1 1 d . . . . .
O21 O 0.5881(6) 0.5519(5) 0.0409(3) 0.0250(12) Uani 1 1 d . . . . .
O22 O 0.5595(6) 0.6646(5) 0.3068(3) 0.0278(13) Uani 1 1 d . . . . .
O30 O -0.1422(6) 0.9505(6) 0.2906(4) 0.0377(15) Uani 1 1 d . . . . .
O31 O -0.0772(7) 0.5473(6) 0.3794(4) 0.0393(15) Uani 1 1 d . . . . .
O32 O 0.2590(6) 0.6994(6) 0.4462(4) 0.0334(14) Uani 1 1 d . . . . .
O40 O 0.3942(7) 0.4314(6) 0.5085(4) 0.0380(15) Uani 1 1 d . . . . .
O41 O 0.7792(7) 0.0603(6) 0.4649(4) 0.0399(16) Uani 1 1 d . . . . .
O42 O 0.7590(7) 0.3964(6) 0.2947(4) 0.0431(16) Uani 1 1 d . . . . .
O50 O 0.1020(8) 0.0921(7) 0.2237(5) 0.055(2) Uani 1 1 d . . . . .
O51 O 0.0661(8) 0.2382(7) 0.4778(5) 0.056(2) Uani 1 1 d . . . . .
O52 O 0.4930(9) -0.1160(6) 0.4039(4) 0.057(2) Uani 1 1 d . . . . .
O60 O 0.2730(6) 0.2528(5) 0.0485(4) 0.0313(13) Uani 1 1 d . . . . .
O61 O 0.6116(6) -0.0796(5) 0.1865(4) 0.0312(13) Uani 1 1 d . . . . .
O62 O 0.7102(6) 0.2785(5) 0.0893(4) 0.0313(13) Uani 1 1 d . . . . .
C2 C 0.1655(8) 0.5309(6) 0.1906(4) 0.0161(15) Uani 1 1 d . . . . .
C3 C 0.2980(8) 0.5257(6) 0.2231(4) 0.0144(14) Uani 1 1 d . . . . .
C4 C 0.3665(8) 0.3934(7) 0.2688(4) 0.0153(14) Uani 1 1 d . . . . .
C5 C 0.2587(8) 0.3376(7) 0.2667(4) 0.0178(15) Uani 1 1 d . . . . .
C10 C -0.0607(8) 0.8770(8) 0.0811(5) 0.0226(17) Uani 1 1 d . . . . .
C11 C -0.1362(8) 0.6635(7) 0.1409(4) 0.0176(15) Uani 1 1 d . . . . .
C12 C 0.0602(8) 0.6337(7) 0.0036(5) 0.0216(16) Uani 1 1 d . . . . .
C20 C 0.3420(9) 0.8541(7) 0.1136(5) 0.0227(17) Uani 1 1 d . . . . .
C21 C 0.4969(9) 0.5996(7) 0.0883(5) 0.0202(16) Uani 1 1 d . . . . .
C22 C 0.4823(8) 0.6716(7) 0.2537(5) 0.0207(16) Uani 1 1 d . . . . .
C30 C -0.0485(9) 0.8511(8) 0.2881(5) 0.0275(18) Uani 1 1 d . . . . .
C31 C -0.0087(9) 0.6007(8) 0.3437(5) 0.0252(18) Uani 1 1 d . . . . .
C32 C 0.2062(8) 0.6884(7) 0.3867(5) 0.0228(17) Uani 1 1 d . . . . .
C40 C 0.4473(9) 0.3770(8) 0.4518(5) 0.0263(18) Uani 1 1 d . . . . .
C41 C 0.6887(10) 0.1390(8) 0.4275(5) 0.0283(19) Uani 1 1 d . . . . .
C42 C 0.6729(9) 0.3548(8) 0.3182(5) 0.0291(19) Uani 1 1 d . . . . .
C50 C 0.1773(10) 0.1188(9) 0.2652(6) 0.036(2) Uani 1 1 d . . . . .
C51 C 0.1530(11) 0.2072(8) 0.4248(6) 0.036(2) Uani 1 1 d . . . . .
C52 C 0.4167(11) -0.0158(8) 0.3776(5) 0.034(2) Uani 1 1 d . . . . .
C60 C 0.3467(8) 0.2387(7) 0.1054(5) 0.0208(16) Uani 1 1 d . . . . .
C61 C 0.5622(8) 0.0287(8) 0.1903(5) 0.0223(17) Uani 1 1 d . . . . .
C62 C 0.6186(8) 0.2582(7) 0.1288(5) 0.0216(16) Uani 1 1 d . . . . .
H4 H 0.422(8) 0.188(8) 0.403(2) 0.07(3) Uiso 1 1 d D . . . .
H5 H 0.611(4) 0.161(4) 0.282(2) 0.02(2) Uiso 1 1 d D . . . .
H2 H 0.1775 0.7933 0.2245 0.127 Uiso 1 1 d D . . . .
H1 H 0.2171 0.7104 0.0807 0.090 Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 Os2 3.0696(4) . ?
Os1 Os3 2.7783(4) . ?
Os1 C2 2.040(7) . ?
Os1 C10 1.957(8) . ?
Os1 C11 1.896(7) . ?
Os1 C12 1.926(8) . ?
Os1 H1 1.8195 . ?
Os2 Os3 2.8480(4) . ?
Os2 C3 2.131(7) . ?
Os2 C20 1.945(8) . ?
Os2 C21 1.922(8) . ?
Os2 C22 1.916(8) . ?
Os2 H2 1.8512 . ?
Os2 H1 1.8253 . ?
Os3 C2 2.336(7) . ?
Os3 C3 2.310(7) . ?
Os3 C30 1.893(9) . ?
Os3 C31 1.901(8) . ?
Os3 C32 1.915(8) . ?
Os3 H2 1.7355 . ?
Os4 Os5 3.0680(5) . ?
Os4 Os6 2.8491(4) . ?
Os4 C4 2.132(7) . ?
Os4 C40 1.927(9) . ?
Os4 C41 1.973(9) . ?
Os4 C42 1.925(9) . ?
Os4 H4 1.79(2) . ?
Os4 HA 1.79(2) . ?
Os5 Os6 2.7666(4) . ?
Os5 C5 2.041(7) . ?
Os5 C50 1.880(10) . ?
Os5 C51 1.920(9) . ?
Os5 C52 1.951(9) . ?
Os5 H4 1.79(2) . ?
Os6 C4 2.320(7) . ?
Os6 C5 2.325(7) . ?
Os6 C60 1.903(8) . ?
Os6 C61 1.907(8) . ?
Os6 C62 1.924(8) . ?
Os6 HA 1.80(2) . ?
O5 C2 1.405(8) . ?
O5 C5 1.397(8) . ?
O10 C10 1.133(9) . ?
O11 C11 1.132(8) . ?
O12 C12 1.133(9) . ?
O20 C20 1.129(9) . ?
O21 C21 1.132(9) . ?
O22 C22 1.134(9) . ?
O30 C30 1.148(10) . ?
O31 C31 1.138(9) . ?
O32 C32 1.138(9) . ?
O40 C40 1.127(9) . ?
O41 C41 1.118(9) . ?
O42 C42 1.128(10) . ?
O50 C50 1.154(11) . ?
O51 C51 1.134(10) . ?
O52 C52 1.134(10) . ?
O60 C60 1.140(9) . ?
O61 C61 1.139(9) . ?
O62 C62 1.131(9) . ?
C2 C3 1.392(10) . ?
C3 C4 1.493(9) . ?
C4 C5 1.415(10) . ?

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
Os2 Os1 H1 32.7 . . ?
Os3 Os1 Os2 58.033(9) . . ?
Os3 Os1 H1 90.2 . . ?
C2 Os1 Os2 65.6(2) . . ?
C2 Os1 Os3 55.48(19) . . ?
C2 Os1 H1 87.5 . . ?
C10 Os1 Os2 100.2(2) . . ?
C10 Os1 Os3 102.3(2) . . ?
C10 Os1 C2 157.3(3) . . ?
C10 Os1 H1 88.4 . . ?
C11 Os1 Os2 151.4(2) . . ?
C11 Os1 Os3 94.8(2) . . ?
C11 Os1 C2 92.5(3) . . ?
C11 Os1 C10 93.9(3) . . ?
C11 Os1 C12 92.1(3) . . ?
C11 Os1 H1 173.9 . . ?
C12 Os1 Os2 110.2(2) . . ?
C12 Os1 Os3 158.0(2) . . ?
C12 Os1 C2 103.4(3) . . ?
C12 Os1 C10 98.0(3) . . ?
C12 Os1 H1 82.0 . . ?
Os1 Os2 H2 64.0 . . ?
Os1 Os2 H1 32.6 . . ?
Os3 Os2 Os1 55.853(10) . . ?
Os3 Os2 H2 36.0 . . ?
Os3 Os2 H1 87.9 . . ?
C3 Os2 Os1 66.67(18) . . ?
C3 Os2 Os3 52.94(18) . . ?
C3 Os2 H2 88.9 . . ?
C3 Os2 H1 89.6 . . ?
C20 Os2 Os1 102.4(2) . . ?
C20 Os2 Os3 118.2(2) . . ?
C20 Os2 C3 168.4(3) . . ?
C20 Os2 H2 82.3 . . ?
C20 Os2 H1 82.3 . . ?
C21 Os2 Os1 109.5(2) . . ?
C21 Os2 Os3 148.7(2) . . ?
C21 Os2 C3 96.6(3) . . ?
C21 Os2 C20 90.9(3) . . ?
C21 Os2 H2 169.0 . . ?
C21 Os2 H1 84.6 . . ?
C22 Os2 Os1 150.5(2) . . ?
C22 Os2 Os3 94.9(2) . . ?
C22 Os2 C3 93.4(3) . . ?
C22 Os2 C20 95.0(3) . . ?
C22 Os2 C21 93.7(3) . . ?
C22 Os2 H2 95.5 . . ?
C22 Os2 H1 176.7 . . ?
H2 Os2 H1 85.9 . . ?
Os1 Os3 Os2 66.114(10) . . ?
Os1 Os3 H2 72.8 . . ?
Os2 Os3 H2 38.9 . . ?
C2 Os3 Os1 46.02(17) . . ?
C2 Os3 Os2 67.24(17) . . ?
C2 Os3 H2 99.0 . . ?
C3 Os3 Os1 70.56(17) . . ?
C3 Os3 Os2 47.40(17) . . ?
C3 Os3 C2 34.9(2) . . ?
C3 Os3 H2 86.2 . . ?
C30 Os3 Os1 88.8(2) . . ?
C30 Os3 Os2 113.9(3) . . ?
C30 Os3 C2 132.1(3) . . ?
C30 Os3 C3 156.2(3) . . ?
C30 Os3 C31 92.5(3) . . ?
C30 Os3 C32 97.7(3) . . ?
C30 Os3 H2 76.2 . . ?
C31 Os3 Os1 101.9(2) . . ?
C31 Os3 Os2 149.8(2) . . ?
C31 Os3 C2 84.4(3) . . ?
C31 Os3 C3 103.0(3) . . ?
C31 Os3 C32 93.4(3) . . ?
C31 Os3 H2 167.4 . . ?
C32 Os3 Os1 163.1(2) . . ?
C32 Os3 Os2 97.0(2) . . ?
C32 Os3 C2 130.1(3) . . ?
C32 Os3 C3 99.2(3) . . ?
C32 Os3 H2 93.6 . . ?
Os5 Os4 H4 31.1(8) . . ?
Os5 Os4 HA 73.6(19) . . ?
Os6 Os4 Os5 55.604(10) . . ?
Os6 Os4 H4 84.6(13) . . ?
Os6 Os4 HA 37.7(7) . . ?
C4 Os4 Os5 67.20(19) . . ?
C4 Os4 Os6 53.18(18) . . ?
C4 Os4 H4 93.0(19) . . ?
C4 Os4 HA 89.9(8) . . ?
C40 Os4 Os5 101.8(2) . . ?
C40 Os4 Os6 145.1(2) . . ?
C40 Os4 C4 95.2(3) . . ?
C40 Os4 C41 94.5(3) . . ?
C40 Os4 H4 83(3) . . ?
C40 Os4 HA 171(2) . . ?
C41 Os4 Os5 104.9(2) . . ?
C41 Os4 Os6 115.8(2) . . ?
C41 Os4 C4 168.6(3) . . ?
C41 Os4 H4 82(2) . . ?
C41 Os4 HA 79.7(9) . . ?
C42 Os4 Os5 154.2(2) . . ?
C42 Os4 Os6 99.1(2) . . ?
C42 Os4 C4 94.3(3) . . ?
C42 Os4 C40 97.5(3) . . ?
C42 Os4 C41 90.3(3) . . ?
C42 Os4 H4 173(2) . . ?
C42 Os4 HA 89(2) . . ?
H4 Os4 HA 90(4) . . ?
Os4 Os5 H4 31.0(8) . . ?
Os6 Os5 Os4 58.186(10) . . ?
Os6 Os5 H4 87.0(13) . . ?
C5 Os5 Os4 65.9(2) . . ?
C5 Os5 Os6 55.4(2) . . ?
C5 Os5 H4 91(2) . . ?
C50 Os5 Os4 152.1(3) . . ?
C50 Os5 Os6 94.8(3) . . ?
C50 Os5 C5 94.0(3) . . ?
C50 Os5 C51 94.0(4) . . ?
C50 Os5 C52 95.3(4) . . ?
C50 Os5 H4 175(2) . . ?
C51 Os5 Os4 108.2(3) . . ?
C51 Os5 Os6 155.2(3) . . ?
C51 Os5 C5 100.9(3) . . ?
C51 Os5 C52 99.6(4) . . ?
C51 Os5 H4 86(2) . . ?
C52 Os5 Os4 97.4(3) . . ?
C52 Os5 Os6 102.6(2) . . ?
C52 Os5 C5 156.8(3) . . ?
C52 Os5 H4 80(3) . . ?
Os4 Os6 HA 37.4(7) . . ?
Os5 Os6 Os4 66.211(11) . . ?
Os5 Os6 HA 82(2) . . ?
C4 Os6 Os4 47.35(17) . . ?
C4 Os6 Os5 71.14(17) . . ?
C4 Os6 C5 35.5(2) . . ?
C4 Os6 HA 83.9(8) . . ?
C5 Os6 Os4 67.54(17) . . ?
C5 Os6 Os5 46.26(17) . . ?
C5 Os6 HA 102.9(10) . . ?
C60 Os6 Os4 150.3(2) . . ?
C60 Os6 Os5 100.7(2) . . ?
C60 Os6 C4 103.9(3) . . ?
C60 Os6 C5 84.1(3) . . ?
C60 Os6 C61 92.6(3) . . ?
C60 Os6 C62 93.2(3) . . ?
C60 Os6 HA 172.2(8) . . ?
C61 Os6 Os4 112.7(2) . . ?
C61 Os6 Os5 88.6(2) . . ?
C61 Os6 C4 155.7(3) . . ?
C61 Os6 C5 132.5(3) . . ?
C61 Os6 C62 97.9(3) . . ?
C61 Os6 HA 80.0(13) . . ?
C62 Os6 Os4 98.2(2) . . ?
C62 Os6 Os5 164.4(2) . . ?
C62 Os6 C4 98.8(3) . . ?
C62 Os6 C5 129.6(3) . . ?
C62 Os6 HA 85(2) . . ?
C5 O5 C2 106.0(5) . . ?
Os1 C2 Os3 78.5(2) . . ?
O5 C2 Os1 129.8(5) . . ?
O5 C2 Os3 118.8(4) . . ?
C3 C2 Os1 118.2(5) . . ?
C3 C2 Os3 71.6(4) . . ?
C3 C2 O5 112.0(6) . . ?
Os2 C3 Os3 79.7(2) . . ?
C2 C3 Os2 109.1(5) . . ?
C2 C3 Os3 73.6(4) . . ?
C2 C3 C4 105.2(6) . . ?
C4 C3 Os2 143.8(5) . . ?
C4 C3 Os3 121.7(4) . . ?
Os4 C4 Os6 79.5(2) . . ?
C3 C4 Os4 143.9(5) . . ?
C3 C4 Os6 123.4(4) . . ?
C5 C4 Os4 108.5(5) . . ?
C5 C4 Os6 72.5(4) . . ?
C5 C4 C3 105.3(6) . . ?
Os5 C5 Os6 78.3(2) . . ?
O5 C5 Os5 130.9(5) . . ?
O5 C5 Os6 119.1(4) . . ?
O5 C5 C4 111.0(6) . . ?
C4 C5 Os5 118.1(5) . . ?
C4 C5 Os6 72.1(4) . . ?
O10 C10 Os1 176.2(7) . . ?
O11 C11 Os1 178.3(6) . . ?
O12 C12 Os1 176.9(7) . . ?
O20 C20 Os2 178.3(7) . . ?
O21 C21 Os2 177.0(6) . . ?
O22 C22 Os2 177.1(7) . . ?
O30 C30 Os3 178.9(7) . . ?
O31 C31 Os3 179.1(8) . . ?
O32 C32 Os3 174.3(7) . . ?
O40 C40 Os4 176.3(8) . . ?
O41 C41 Os4 178.0(7) . . ?
O42 C42 Os4 177.3(7) . . ?
O50 C50 Os5 179.5(9) . . ?
O51 C51 Os5 177.7(8) . . ?
O52 C52 Os5 175.1(9) . . ?
O60 C60 Os6 177.8(7) . . ?
O61 C61 Os6 178.2(7) . . ?
O62 C62 Os6 175.2(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_p21c
_audit_block_doi                 10.5517/ccdc.csd.cc1z50v0
_database_code_depnum_ccdc_archive 'CCDC 1822082'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8CC01532E 2018
_audit_update_record             
;
2018-02-03 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H4 O20 Os6'
_chemical_formula_weight         1741.46

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   14.0260(7)
_cell_length_b                   9.5121(5)
_cell_length_c                   24.6707(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.081(2)
_cell_angle_gamma                90.00
_cell_volume                     3273.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9704
_cell_measurement_theta_min      4.593
_cell_measurement_theta_max      56.450

_exptl_crystal_description       plate
_exptl_crystal_colour            yelloq
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3032
_exptl_absorpt_coefficient_mu    23.284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0787
_exptl_absorpt_correction_T_max  0.1688
_exptl_absorpt_process_details   '(SADABS, Bruker, 2016)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            117503
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         28.37
_reflns_number_total             8189
_reflns_number_gt                6804
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0206P)²+22.2771P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8189
_refine_ls_number_parameters     450
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0551
_refine_ls_wR_factor_gt          0.0512
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.181809(17) 0.58447(3) 0.224148(10) 0.01302(6) Uani 1 1 d . . .
Os2 Os 0.275526(18) 0.30108(3) 0.221616(10) 0.01628(6) Uani 1 1 d . . .
Os3 Os 0.365950(18) 0.54622(3) 0.189825(10) 0.01534(6) Uani 1 1 d . . .
Os4 Os 0.167345(18) 0.42629(3) 0.426727(10) 0.01623(6) Uani 1 1 d . . .
Os5 Os 0.311255(18) 0.56876(3) 0.494691(10) 0.01808(6) Uani 1 1 d . . .
Os6 Os 0.196267(18) 0.72674(3) 0.412473(10) 0.01495(6) Uani 1 1 d . . .
O5 O 0.2433(3) 0.4700(5) 0.35894(17) 0.0153(9) Uani 1 1 d . . .
O10 O 0.0853(4) 0.5119(5) 0.11111(19) 0.0255(11) Uani 1 1 d . . .
O11 O -0.0074(3) 0.5907(5) 0.2762(2) 0.0277(12) Uani 1 1 d . . .
O12 O 0.1844(4) 0.8990(5) 0.1977(2) 0.0269(11) Uani 1 1 d . . .
O20 O 0.1411(5) 0.1794(6) 0.1257(3) 0.0490(17) Uani 1 1 d . . .
O21 O 0.2226(4) 0.1037(6) 0.3108(2) 0.0332(13) Uani 1 1 d . . .
O22 O 0.4481(4) 0.1364(5) 0.1922(2) 0.0310(12) Uani 1 1 d . . .
O30 O 0.2963(4) 0.4652(6) 0.0720(2) 0.0357(13) Uani 1 1 d . . .
O31 O 0.3965(4) 0.8546(6) 0.1624(2) 0.0353(13) Uani 1 1 d . . .
O32 O 0.5759(4) 0.4602(6) 0.1946(2) 0.0366(14) Uani 1 1 d . . .
O40 O 0.0183(4) 0.2876(6) 0.3444(2) 0.0408(15) Uani 1 1 d . . .
O41 O 0.0489(4) 0.3657(7) 0.5191(2) 0.0382(14) Uani 1 1 d . . .
O42 O 0.2772(5) 0.1560(6) 0.4537(2) 0.0414(14) Uani 1 1 d . . .
O50 O 0.1563(4) 0.6446(7) 0.5696(2) 0.0437(15) Uani 1 1 d . . .
O51 O 0.4511(4) 0.7950(6) 0.5429(2) 0.0380(14) Uani 1 1 d . . .
O52 O 0.3826(4) 0.3235(6) 0.5680(2) 0.0440(15) Uani 1 1 d . . .
O53 O 0.4422(3) 0.4896(6) 0.4063(2) 0.0308(12) Uani 1 1 d . . .
O60 O 0.0705(4) 0.8818(5) 0.3234(2) 0.0279(12) Uani 1 1 d . . .
O61 O 0.0969(4) 0.8996(7) 0.4976(2) 0.0421(15) Uani 1 1 d . . .
O62 O 0.3740(4) 0.9128(5) 0.4153(2) 0.0299(12) Uani 1 1 d . . .
C2 C 0.3647(5) 0.4302(7) 0.2702(3) 0.0177(14) Uani 1 1 d D . .
C3 C 0.3303(4) 0.5660(7) 0.2697(3) 0.0147(13) Uani 1 1 d . . .
C4 C 0.2796(4) 0.6541(6) 0.3017(3) 0.0143(13) Uani 1 1 d . . .
C5 C 0.2478(4) 0.6036(6) 0.3534(2) 0.0117(12) Uani 1 1 d . . .
C10 C 0.1211(5) 0.5386(7) 0.1535(3) 0.0196(14) Uani 1 1 d . . .
C11 C 0.0628(5) 0.5884(7) 0.2575(3) 0.0194(14) Uani 1 1 d . . .
C12 C 0.1833(5) 0.7824(7) 0.2074(3) 0.0195(14) Uani 1 1 d . . .
C20 C 0.1894(6) 0.2237(7) 0.1612(3) 0.0279(17) Uani 1 1 d . . .
C21 C 0.2401(5) 0.1754(7) 0.2757(3) 0.0228(15) Uani 1 1 d . . .
C22 C 0.3822(6) 0.1931(7) 0.2031(3) 0.0242(16) Uani 1 1 d . . .
C30 C 0.3256(5) 0.4920(7) 0.1153(3) 0.0225(15) Uani 1 1 d . . .
C31 C 0.3855(5) 0.7385(7) 0.1736(3) 0.0215(15) Uani 1 1 d . . .
C32 C 0.4977(5) 0.4918(8) 0.1903(3) 0.0254(16) Uani 1 1 d . . .
C40 C 0.0721(5) 0.3441(8) 0.3749(3) 0.0259(16) Uani 1 1 d . . .
C41 C 0.0938(5) 0.3914(8) 0.4848(3) 0.0235(15) Uani 1 1 d . . .
C42 C 0.2367(6) 0.2582(8) 0.4435(3) 0.0279(17) Uani 1 1 d . . .
C50 C 0.2130(5) 0.6167(9) 0.5413(3) 0.0281(17) Uani 1 1 d . . .
C51 C 0.3986(5) 0.7126(8) 0.5253(3) 0.0258(16) Uani 1 1 d . . .
C52 C 0.3566(5) 0.4134(8) 0.5411(3) 0.0275(17) Uani 1 1 d . . .
C53 C 0.3930(5) 0.5197(8) 0.4378(3) 0.0237(15) Uani 1 1 d . . .
C60 C 0.1163(5) 0.8221(7) 0.3566(3) 0.0197(14) Uani 1 1 d . . .
C61 C 0.1349(5) 0.8337(8) 0.4684(3) 0.0275(17) Uani 1 1 d . . .
C62 C 0.3060(5) 0.8469(8) 0.4144(3) 0.0237(15) Uani 1 1 d . . .
H1 H 0.1786 0.4023 0.2437 0.000 Uiso 1 1 d . . .
H2 H 0.415(3) 0.414(7) 0.295(2) 0.013(17) Uiso 1 1 d D . .
H4 H 0.2818 0.7463 0.2979 0.004 Uiso 1 1 d . . .
H5 H 0.119(6) 0.582(9) 0.417(4) 0.05(3) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C10 1.908(7) . ?
Os1 C12 1.928(7) . ?
Os1 C11 1.938(7) . ?
Os1 C3 2.267(6) . ?
Os1 C4 2.329(6) . ?
Os1 Os3 2.8255(4) . ?
Os1 Os2 3.0026(4) . ?
Os1 H1 1.8008 . ?
Os2 C21 1.897(7) . ?
Os2 C22 1.910(7) . ?
Os2 C20 1.960(8) . ?
Os2 C2 2.048(7) . ?
Os2 Os3 2.8056(4) . ?
Os2 H1 1.7966 . ?
Os3 C31 1.898(7) . ?
Os3 C32 1.917(7) . ?
Os3 C30 1.937(8) . ?
Os3 C3 2.092(6) . ?
Os3 C2 2.272(7) . ?
Os4 C41 1.882(7) . ?
Os4 C42 1.895(8) . ?
Os4 C40 1.916(7) . ?
Os4 O5 2.117(4) . ?
Os4 Os5 2.8293(4) . ?
Os4 Os6 2.9131(4) . ?
Os4 H5 1.63(9) . ?
Os5 C52 1.934(8) . ?
Os5 C51 1.936(8) . ?
Os5 C50 1.941(8) . ?
Os5 C53 1.960(8) . ?
Os5 Os6 2.8776(4) . ?
Os6 C60 1.912(7) . ?
Os6 C62 1.913(7) . ?
Os6 C61 1.983(8) . ?
Os6 C5 2.058(6) . ?
Os6 H5 1.77(9) . ?
O5 C5 1.280(7) . ?
O10 C10 1.140(8) . ?
O11 C11 1.131(8) . ?
O12 C12 1.135(8) . ?
O20 C20 1.131(9) . ?
O21 C21 1.149(8) . ?
O22 C22 1.127(8) . ?
O30 C30 1.132(9) . ?
O31 C31 1.153(8) . ?
O32 C32 1.132(8) . ?
O40 C40 1.142(9) . ?
O41 C41 1.134(8) . ?
O42 C42 1.140(9) . ?
O50 C50 1.143(9) . ?
O51 C51 1.130(9) . ?
O52 C52 1.121(9) . ?
O53 C53 1.129(8) . ?
O60 C60 1.137(8) . ?
O61 C61 1.129(9) . ?
O62 C62 1.140(8) . ?
C2 C3 1.379(9) . ?
C2 H2 0.89(2) . ?
C3 C4 1.398(9) . ?
C4 C5 1.476(8) . ?
C4 H4 0.8825 . ?

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
C10 Os1 C12 92.4(3) . . ?
C10 Os1 C11 94.1(3) . . ?
C12 Os1 C11 95.8(3) . . ?
C10 Os1 C3 137.1(3) . . ?
C12 Os1 C3 98.7(3) . . ?
C11 Os1 C3 125.4(3) . . ?
C10 Os1 C4 169.3(2) . . ?
C12 Os1 C4 83.1(3) . . ?
C11 Os1 C4 96.0(2) . . ?
C3 Os1 C4 35.4(2) . . ?
C10 Os1 Os3 91.7(2) . . ?
C12 Os1 Os3 91.7(2) . . ?
C11 Os1 Os3 170.2(2) . . ?
C3 Os1 Os3 46.95(16) . . ?
C4 Os1 Os3 78.80(15) . . ?
C10 Os1 Os2 86.0(2) . . ?
C12 Os1 Os2 149.0(2) . . ?
C11 Os1 Os2 115.1(2) . . ?
C3 Os1 Os2 63.85(16) . . ?
C4 Os1 Os2 92.96(15) . . ?
Os3 Os1 Os2 57.458(8) . . ?
C10 Os1 H1 90.2 . . ?
C12 Os1 H1 176.6 . . ?
C11 Os1 H1 81.8 . . ?
C3 Os1 H1 80.8 . . ?
C4 Os1 H1 94.7 . . ?
Os3 Os1 H1 90.3 . . ?
Os2 Os1 H1 33.4 . . ?
C21 Os2 C22 95.7(3) . . ?
C21 Os2 C20 96.4(3) . . ?
C22 Os2 C20 92.9(3) . . ?
C21 Os2 C2 98.9(3) . . ?
C22 Os2 C2 91.0(3) . . ?
C20 Os2 C2 163.7(3) . . ?
C21 Os2 Os3 151.7(2) . . ?
C22 Os2 Os3 89.5(2) . . ?
C20 Os2 Os3 111.1(2) . . ?
C2 Os2 Os3 53.06(18) . . ?
C21 Os2 Os1 113.8(2) . . ?
C22 Os2 Os1 147.5(2) . . ?
C20 Os2 Os1 96.7(2) . . ?
C2 Os2 Os1 72.01(18) . . ?
Os3 Os2 Os1 58.098(9) . . ?
C21 Os2 H1 82.0 . . ?
C22 Os2 H1 176.2 . . ?
C20 Os2 H1 90.4 . . ?
C2 Os2 H1 86.3 . . ?
Os3 Os2 H1 91.1 . . ?
Os1 Os2 H1 33.5 . . ?
C31 Os3 C32 95.8(3) . . ?
C31 Os3 C30 95.2(3) . . ?
C32 Os3 C30 96.8(3) . . ?
C31 Os3 C3 99.5(3) . . ?
C32 Os3 C3 110.2(3) . . ?
C30 Os3 C3 147.5(3) . . ?
C31 Os3 C2 131.8(3) . . ?
C32 Os3 C2 87.7(3) . . ?
C30 Os3 C2 132.2(3) . . ?
C3 Os3 C2 36.5(2) . . ?
C31 Os3 Os2 159.9(2) . . ?
C32 Os3 Os2 103.7(2) . . ?
C30 Os3 Os2 87.1(2) . . ?
C3 Os3 Os2 69.58(17) . . ?
C2 Os3 Os2 46.09(17) . . ?
C31 Os3 Os1 95.5(2) . . ?
C32 Os3 Os1 160.7(2) . . ?
C30 Os3 Os1 97.7(2) . . ?
C3 Os3 Os1 52.34(16) . . ?
C2 Os3 Os1 73.09(17) . . ?
Os2 Os3 Os1 64.444(9) . . ?
C41 Os4 C42 89.8(3) . . ?
C41 Os4 C40 92.1(3) . . ?
C42 Os4 C40 96.1(3) . . ?
C41 Os4 O5 176.9(2) . . ?
C42 Os4 O5 92.8(2) . . ?
C40 Os4 O5 85.8(2) . . ?
C41 Os4 Os5 92.7(2) . . ?
C42 Os4 Os5 87.6(2) . . ?
C40 Os4 Os5 173.9(2) . . ?
O5 Os4 Os5 89.25(12) . . ?
C41 Os4 Os6 111.1(2) . . ?
C42 Os4 Os6 141.2(2) . . ?
C40 Os4 Os6 114.6(2) . . ?
O5 Os4 Os6 67.89(12) . . ?
Os5 Os4 Os6 60.126(9) . . ?
C41 Os4 H5 91(3) . . ?
C42 Os4 H5 173(3) . . ?
C40 Os4 H5 91(3) . . ?
O5 Os4 H5 87(3) . . ?
Os5 Os4 H5 85(3) . . ?
Os6 Os4 H5 32(3) . . ?
C52 Os5 C51 98.9(3) . . ?
C52 Os5 C50 92.2(3) . . ?
C51 Os5 C50 93.6(3) . . ?
C52 Os5 C53 93.5(3) . . ?
C51 Os5 C53 93.1(3) . . ?
C50 Os5 C53 170.5(3) . . ?
C52 Os5 Os4 98.8(2) . . ?
C51 Os5 Os4 162.2(2) . . ?
C50 Os5 Os4 87.5(2) . . ?
C53 Os5 Os4 84.1(2) . . ?
C52 Os5 Os6 160.1(2) . . ?
C51 Os5 Os6 101.0(2) . . ?
C50 Os5 Os6 85.1(2) . . ?
C53 Os5 Os6 86.9(2) . . ?
Os4 Os5 Os6 61.381(9) . . ?
C60 Os6 C62 98.2(3) . . ?
C60 Os6 C61 89.7(3) . . ?
C62 Os6 C61 94.8(3) . . ?
C60 Os6 C5 89.0(3) . . ?
C62 Os6 C5 90.9(3) . . ?
C61 Os6 C5 174.3(3) . . ?
C60 Os6 Os5 176.8(2) . . ?
C62 Os6 Os5 84.6(2) . . ?
C61 Os6 Os5 91.7(2) . . ?
C5 Os6 Os5 89.37(16) . . ?
C60 Os6 Os4 118.3(2) . . ?
C62 Os6 Os4 134.8(2) . . ?
C61 Os6 Os4 110.0(2) . . ?
C5 Os6 Os4 65.86(17) . . ?
Os5 Os6 Os4 58.493(9) . . ?
C60 Os6 H5 96(3) . . ?
C62 Os6 H5 164(3) . . ?
C61 Os6 H5 92(3) . . ?
C5 Os6 H5 82(3) . . ?
Os5 Os6 H5 81(3) . . ?
Os4 Os6 H5 30(3) . . ?
C5 O5 Os4 108.3(4) . . ?
C3 C2 Os2 111.4(4) . . ?
C3 C2 Os3 64.6(4) . . ?
Os2 C2 Os3 80.8(2) . . ?
C3 C2 H2 115(4) . . ?
Os2 C2 H2 133(4) . . ?
Os3 C2 H2 127(4) . . ?
C2 C3 C4 139.1(6) . . ?
C2 C3 Os3 78.8(4) . . ?
C4 C3 Os3 140.6(5) . . ?
C2 C3 Os1 112.3(4) . . ?
C4 C3 Os1 74.8(4) . . ?
Os3 C3 Os1 80.7(2) . . ?
C3 C4 C5 120.8(6) . . ?
C3 C4 Os1 69.9(3) . . ?
C5 C4 Os1 114.4(4) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 115.7 . . ?
Os1 C4 H4 102.6 . . ?
O5 C5 C4 115.9(5) . . ?
O5 C5 Os6 117.7(4) . . ?
C4 C5 Os6 126.0(4) . . ?
O10 C10 Os1 179.5(7) . . ?
O11 C11 Os1 179.0(6) . . ?
O12 C12 Os1 179.8(8) . . ?
O20 C20 Os2 178.6(7) . . ?
O21 C21 Os2 175.7(6) . . ?
O22 C22 Os2 176.0(7) . . ?
O30 C30 Os3 175.3(6) . . ?
O31 C31 Os3 178.2(7) . . ?
O32 C32 Os3 175.0(7) . . ?
O40 C40 Os4 175.9(7) . . ?
O41 C41 Os4 177.5(7) . . ?
O42 C42 Os4 178.9(7) . . ?
O50 C50 Os5 178.8(7) . . ?
O51 C51 Os5 178.6(7) . . ?
O52 C52 Os5 179.8(8) . . ?
O53 C53 Os5 177.8(6) . . ?
O60 C60 Os6 178.1(6) . . ?
O61 C61 Os6 175.5(7) . . ?
O62 C62 Os6 176.6(6) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.421
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.267
####################################################################### 
# 
# 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_jkos3fur1_0m
_audit_block_doi                 10.5517/ccdc.csd.cc1z50qw
_database_code_depnum_ccdc_archive 'CCDC 1822078'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8CC01532E 2018
_audit_update_record             
;
2018-02-03 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H4 O20 Os6'
_chemical_formula_weight         1741.46

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.3105(5)
_cell_length_b                   16.1718(8)
_cell_length_c                   18.3462(8)
_cell_angle_alpha                87.0138(14)
_cell_angle_beta                 89.5808(15)
_cell_angle_gamma                81.0114(15)
_cell_volume                     3310.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9796
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.63

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3032
_exptl_absorpt_coefficient_mu    23.023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1687
_exptl_absorpt_correction_T_max  0.6560
_exptl_absorpt_process_details   '(SADABS, Bruker, 2016)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            85196
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         27.63
_reflns_number_total             15344
_reflns_number_gt                12620
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0191P)²+30.7442P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15344
_refine_ls_number_parameters     899
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0646
_refine_ls_wR_factor_gt          0.0599
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.183
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.81356(3) 0.62675(2) 0.131607(18) 0.01414(7) Uani 1 1 d D . .
Os2 Os 0.71994(3) 0.71394(2) 0.270753(18) 0.01392(7) Uani 1 1 d D . .
Os3 Os 0.77711(3) 0.80371(2) 0.145440(18) 0.01410(7) Uani 1 1 d D . .
Os4 Os 0.37542(3) 0.67962(2) 0.056109(17) 0.01373(7) Uani 1 1 d D . .
H5 H 0.4219 0.7279 -0.0269 0.000 Uiso 1 1 d D . .
Os5 Os 0.28791(3) 0.85251(2) 0.077434(18) 0.01287(7) Uani 1 1 d . . .
Os6 Os 0.29475(3) 0.79342(2) -0.065703(18) 0.01382(7) Uani 1 1 d D . .
Os7 Os -0.14854(3) 0.63131(2) 0.637705(18) 0.01336(7) Uani 1 1 d D . .
Os8 Os -0.10125(3) 0.72625(2) 0.773026(17) 0.01295(7) Uani 1 1 d D . .
Os9 Os -0.19282(3) 0.80926(2) 0.644465(18) 0.01295(7) Uani 1 1 d D . .
Os10 Os 0.27129(3) 0.67951(2) 0.563972(17) 0.01301(7) Uani 1 1 d D . .
H5A H 0.3613 0.6898 0.4873 0.113 Uiso 1 1 d D . .
Os11 Os 0.27913(3) 0.85388(2) 0.577321(17) 0.01196(7) Uani 1 1 d . . .
Os12 Os 0.30254(3) 0.78697(2) 0.437157(17) 0.01311(7) Uani 1 1 d D . .
O5 O 0.4933(5) 0.7838(4) 0.1743(3) 0.0155(13) Uani 1 1 d . . .
O5A O 0.0989(5) 0.7911(3) 0.6753(3) 0.0129(12) Uani 1 1 d . . .
O10 O 1.0573(6) 0.5284(4) 0.1829(4) 0.0306(17) Uani 1 1 d . . .
O11 O 0.8710(7) 0.6148(4) -0.0304(4) 0.0301(16) Uani 1 1 d . . .
O12 O 0.6722(6) 0.4810(4) 0.1233(4) 0.0243(15) Uani 1 1 d . . .
O20 O 0.9581(6) 0.7029(4) 0.3542(4) 0.0296(17) Uani 1 1 d . . .
O21 O 0.5968(7) 0.5908(4) 0.3650(4) 0.0311(17) Uani 1 1 d . . .
O22 O 0.6108(6) 0.8729(4) 0.3431(4) 0.0297(16) Uani 1 1 d . . .
O30 O 0.9832(7) 0.8693(5) 0.2194(4) 0.0333(17) Uani 1 1 d . . .
O31 O 0.8163(6) 0.8448(4) -0.0174(4) 0.0286(16) Uani 1 1 d . . .
O32 O 0.6007(6) 0.9630(4) 0.1670(4) 0.0267(15) Uani 1 1 d . . .
O40 O 0.4560(6) 0.5773(4) 0.1975(3) 0.0237(15) Uani 1 1 d . . .
O41 O 0.5480(6) 0.5754(4) -0.0439(4) 0.0248(15) Uani 1 1 d . . .
O42 O 0.1866(6) 0.5698(4) 0.0322(4) 0.0263(15) Uani 1 1 d . . .
O50 O 0.0226(6) 0.9215(4) 0.0489(4) 0.0247(15) Uani 1 1 d . . .
O51 O 0.2575(7) 0.9022(5) 0.2356(4) 0.0374(19) Uani 1 1 d . . .
O52 O 0.3686(6) 1.0112(4) 0.0126(4) 0.0307(17) Uani 1 1 d . . .
O60 O 0.5335(6) 0.8631(4) -0.0913(3) 0.0230(15) Uani 1 1 d . . .
O61 O 0.3434(7) 0.6915(5) -0.2020(4) 0.0371(19) Uani 1 1 d . . .
O62 O 0.1611(6) 0.9597(4) -0.1309(3) 0.0234(15) Uani 1 1 d . . .
O63 O 0.0536(6) 0.7408(4) -0.0200(4) 0.0233(15) Uani 1 1 d . . .
O70 O -0.3455(7) 0.5302(5) 0.6904(4) 0.0392(19) Uani 1 1 d . . .
O71 O 0.0527(6) 0.4816(4) 0.6406(4) 0.0287(16) Uani 1 1 d . . .
O72 O -0.1958(6) 0.6160(4) 0.4758(3) 0.0265(15) Uani 1 1 d . . .
O80 O -0.3309(6) 0.7042(5) 0.8587(4) 0.0350(18) Uani 1 1 d . . .
O81 O 0.0860(6) 0.6145(4) 0.8675(3) 0.0264(16) Uani 1 1 d . . .
O82 O -0.0729(7) 0.8902(4) 0.8404(4) 0.0305(16) Uani 1 1 d . . .
O90 O -0.4305(6) 0.8771(5) 0.7164(4) 0.0323(17) Uani 1 1 d . . .
O91 O -0.0891(6) 0.9697(4) 0.6621(4) 0.0264(15) Uani 1 1 d . . .
O92 O -0.2435(6) 0.8427(4) 0.4806(3) 0.0268(16) Uani 1 1 d . . .
O100 O 0.2306(6) 0.5802(4) 0.7060(4) 0.0261(15) Uani 1 1 d . . .
O101 O 0.5165(6) 0.5725(4) 0.5475(4) 0.0271(16) Uani 1 1 d . . .
O102 O 0.1585(6) 0.5729(4) 0.4605(4) 0.0308(17) Uani 1 1 d . . .
O110 O 0.2810(6) 0.9112(5) 0.7330(4) 0.0318(17) Uani 1 1 d . . .
O111 O 0.5149(6) 0.9211(4) 0.5448(4) 0.0242(15) Uani 1 1 d . . .
O112 O 0.1264(6) 1.0106(4) 0.5104(4) 0.0255(15) Uani 1 1 d . . .
O120 O 0.5679(6) 0.7350(4) 0.4786(4) 0.0238(15) Uani 1 1 d . . .
O121 O 0.3583(6) 0.9530(4) 0.3687(3) 0.0231(14) Uani 1 1 d . . .
O122 O 0.3026(8) 0.6760(5) 0.3070(4) 0.045(2) Uani 1 1 d . . .
O123 O 0.0356(6) 0.8578(4) 0.4104(3) 0.0226(14) Uani 1 1 d . . .
C2 C 0.6079(8) 0.7397(5) 0.1837(5) 0.0145(18) Uani 1 1 d . . .
C3 C 0.6532(8) 0.7153(5) 0.1152(5) 0.0159(18) Uani 1 1 d . . .
C4 C 0.5594(8) 0.7465(5) 0.0619(5) 0.0154(18) Uani 1 1 d . . .
H4 H 0.5851 0.7737 0.0155 0.019 Uiso 1 1 calc R . .
C5 C 0.4627(8) 0.7905(5) 0.0984(5) 0.0178(19) Uani 1 1 d . . .
C2A C 0.0047(8) 0.7484(5) 0.6851(4) 0.0125(17) Uani 1 1 d . . .
C3A C -0.0287(8) 0.7184(5) 0.6194(5) 0.0139(17) Uani 1 1 d . . .
C4A C 0.0553(8) 0.7461(5) 0.5653(5) 0.0167(18) Uani 1 1 d . . .
H4A H 0.0203 0.7705 0.5176 0.020 Uiso 1 1 calc R . .
C5A C 0.1321(7) 0.7924(5) 0.6001(4) 0.0119(17) Uani 1 1 d . . .
C10 C 0.9688(9) 0.5625(6) 0.1627(5) 0.022(2) Uani 1 1 d . . .
C11 C 0.8502(8) 0.6206(5) 0.0302(5) 0.0185(19) Uani 1 1 d . . .
C12 C 0.7277(8) 0.5331(6) 0.1276(5) 0.0178(19) Uani 1 1 d . . .
C20 C 0.8705(9) 0.7054(5) 0.3248(5) 0.019(2) Uani 1 1 d . . .
C21 C 0.6454(8) 0.6357(6) 0.3307(5) 0.021(2) Uani 1 1 d . . .
C22 C 0.6525(9) 0.8118(6) 0.3167(5) 0.022(2) Uani 1 1 d . . .
C30 C 0.9043(10) 0.8467(6) 0.1911(5) 0.025(2) Uani 1 1 d . . .
C31 C 0.8043(8) 0.8323(6) 0.0442(5) 0.022(2) Uani 1 1 d . . .
C32 C 0.6670(9) 0.9048(6) 0.1594(5) 0.021(2) Uani 1 1 d . . .
C40 C 0.4235(7) 0.6174(5) 0.1466(5) 0.0159(18) Uani 1 1 d . . .
C41 C 0.4839(8) 0.6145(5) -0.0076(5) 0.0179(19) Uani 1 1 d . . .
C42 C 0.2549(9) 0.6131(5) 0.0397(5) 0.020(2) Uani 1 1 d . . .
C50 C 0.1203(8) 0.8960(5) 0.0587(5) 0.0163(18) Uani 1 1 d . . .
C51 C 0.2720(9) 0.8813(6) 0.1783(5) 0.023(2) Uani 1 1 d . . .
C52 C 0.3367(8) 0.9527(5) 0.0383(5) 0.020(2) Uani 1 1 d . . .
C60 C 0.4488(9) 0.8345(6) -0.0804(4) 0.020(2) Uani 1 1 d . . .
C61 C 0.3237(8) 0.7268(5) -0.1496(5) 0.0194(19) Uani 1 1 d . . .
C62 C 0.2134(8) 0.8974(6) -0.1088(5) 0.0192(19) Uani 1 1 d . . .
C63 C 0.1437(9) 0.7581(5) -0.0370(5) 0.021(2) Uani 1 1 d . . .
C70 C -0.2734(9) 0.5670(6) 0.6699(5) 0.023(2) Uani 1 1 d . . .
C71 C -0.0233(9) 0.5360(6) 0.6399(5) 0.019(2) Uani 1 1 d . . .
C72 C -0.1784(8) 0.6219(5) 0.5353(5) 0.019(2) Uani 1 1 d . . .
C80 C -0.2448(9) 0.7130(6) 0.8291(5) 0.022(2) Uani 1 1 d . . .
C81 C 0.0139(9) 0.6559(5) 0.8337(5) 0.0187(19) Uani 1 1 d . . .
C82 C -0.0841(8) 0.8294(6) 0.8156(5) 0.0190(19) Uani 1 1 d . . .
C90 C -0.3418(9) 0.8533(6) 0.6886(5) 0.021(2) Uani 1 1 d . . .
C91 C -0.1292(8) 0.9106(6) 0.6555(5) 0.020(2) Uani 1 1 d . . .
C92 C -0.2280(8) 0.8331(5) 0.5411(5) 0.0188(19) Uani 1 1 d . . .
C100 C 0.2453(8) 0.6197(6) 0.6552(5) 0.0190(19) Uani 1 1 d . . .
C101 C 0.4246(9) 0.6136(6) 0.5525(5) 0.021(2) Uani 1 1 d . . .
C102 C 0.2010(8) 0.6131(5) 0.4997(5) 0.0178(19) Uani 1 1 d . . .
C110 C 0.2772(8) 0.8881(6) 0.6763(5) 0.021(2) Uani 1 1 d . . .
C111 C 0.4278(9) 0.8954(5) 0.5567(4) 0.018(2) Uani 1 1 d . . .
C112 C 0.1849(8) 0.9542(6) 0.5359(5) 0.0178(19) Uani 1 1 d . . .
C120 C 0.4701(9) 0.7528(6) 0.4634(5) 0.021(2) Uani 1 1 d . . .
C121 C 0.3385(8) 0.8901(6) 0.3919(5) 0.021(2) Uani 1 1 d . . .
C122 C 0.3052(9) 0.7152(6) 0.3556(5) 0.026(2) Uani 1 1 d . . .
C123 C 0.1333(9) 0.8291(5) 0.4232(5) 0.0178(19) Uani 1 1 d . . .
H1 H 0.783(7) 0.620(2) 0.2281(15) 0.02(2) Uiso 1 1 d D . .
H2 H 0.892(2) 0.7146(17) 0.136(7) 0.07(4) Uiso 1 1 d D . .
H1A H -0.117(9) 0.629(2) 0.7339(16) 0.04(3) Uiso 1 1 d D . .
H2A H -0.268(2) 0.7190(14) 0.644(6) 0.05(3) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C11 1.907(10) . ?
Os1 C12 1.927(10) . ?
Os1 C10 1.968(10) . ?
Os1 C3 2.141(9) . ?
Os1 Os3 2.8512(5) . ?
Os1 Os2 3.0814(5) . ?
Os1 H1 1.80(2) . ?
Os1 H2 1.80(2) . ?
Os2 C22 1.884(10) . ?
Os2 C21 1.923(9) . ?
Os2 C20 1.958(10) . ?
Os2 C2 2.031(9) . ?
Os2 Os3 2.7811(5) . ?
Os2 H1 1.79(2) . ?
Os3 C30 1.909(11) . ?
Os3 C32 1.921(10) . ?
Os3 C31 1.925(10) . ?
Os3 C3 2.245(8) . ?
Os3 C2 2.397(8) . ?
Os3 H2 1.80(2) . ?
Os4 C42 1.899(10) . ?
Os4 C41 1.919(10) . ?
Os4 C40 1.931(9) . ?
Os4 C5 2.346(9) . ?
Os4 C4 2.496(9) . ?
Os4 Os5 2.8624(5) . ?
Os4 Os6 2.8792(5) . ?
Os4 H5 1.7892 . ?
Os5 C52 1.897(9) . ?
Os5 C51 1.931(9) . ?
Os5 C50 1.943(9) . ?
Os5 C5 2.101(9) . ?
Os5 Os6 2.8374(5) . ?
Os6 C62 1.920(9) . ?
Os6 C61 1.921(9) . ?
Os6 C63 1.945(10) . ?
Os6 C60 1.971(11) . ?
Os6 H5 1.7766 . ?
Os7 H2A 1.80(2) . ?
Os7 C71 1.923(10) . ?
Os7 C72 1.930(9) . ?
Os7 C70 1.951(10) . ?
Os7 C3A 2.115(8) . ?
Os7 Os9 2.8519(5) . ?
Os7 Os8 3.0790(5) . ?
Os7 H1A 1.80(2) . ?
Os7 H2A 1.80(2) . ?
Os8 C81 1.912(9) . ?
Os8 C82 1.915(10) . ?
Os8 C80 1.950(10) . ?
Os8 C2A 2.053(8) . ?
Os8 Os9 2.7765(5) . ?
Os8 H1A 1.80(2) . ?
Os9 C91 1.911(10) . ?
Os9 C90 1.915(10) . ?
Os9 C92 1.947(9) . ?
Os9 C3A 2.241(8) . ?
Os9 C2A 2.403(8) . ?
Os9 H2A 1.80(2) . ?
Os10 C102 1.895(9) . ?
Os10 C101 1.905(10) . ?
Os10 C100 1.933(9) . ?
Os10 C5A 2.338(8) . ?
Os10 C4A 2.511(9) . ?
Os10 Os11 2.8583(5) . ?
Os10 Os12 2.8838(5) . ?
Os10 H5A 1.7472 . ?
Os11 C112 1.920(10) . ?
Os11 C110 1.924(9) . ?
Os11 C111 1.934(10) . ?
Os11 C5A 2.096(8) . ?
Os11 Os12 2.8362(5) . ?
Os12 C121 1.923(10) . ?
Os12 C122 1.938(10) . ?
Os12 C123 1.943(10) . ?
Os12 C120 1.946(10) . ?
Os12 H5A 1.8132 . ?
O5 C2 1.386(10) . ?
O5 C5 1.431(10) . ?
O5A C2A 1.363(10) . ?
O5A C5A 1.427(9) . ?
O10 C10 1.120(11) . ?
O11 C11 1.142(11) . ?
O12 C12 1.134(11) . ?
O20 C20 1.126(11) . ?
O21 C21 1.139(11) . ?
O22 C22 1.155(11) . ?
O30 C30 1.153(12) . ?
O31 C31 1.147(11) . ?
O32 C32 1.123(11) . ?
O40 C40 1.138(10) . ?
O41 C41 1.123(11) . ?
O42 C42 1.134(11) . ?
O50 C50 1.129(10) . ?
O51 C51 1.124(11) . ?
O52 C52 1.142(11) . ?
O60 C60 1.139(11) . ?
O61 C61 1.147(11) . ?
O62 C62 1.142(10) . ?
O63 C63 1.136(11) . ?
O70 C70 1.133(11) . ?
O71 C71 1.129(11) . ?
O72 C72 1.122(11) . ?
O80 C80 1.136(11) . ?
O81 C81 1.136(10) . ?
O82 C82 1.131(11) . ?
O90 C90 1.144(11) . ?
O91 C91 1.132(11) . ?
O92 C92 1.123(11) . ?
O100 C100 1.128(10) . ?
O101 C101 1.148(11) . ?
O102 C102 1.149(11) . ?
O110 C110 1.128(11) . ?
O111 C111 1.143(11) . ?
O112 C112 1.123(11) . ?
O120 C120 1.131(11) . ?
O121 C121 1.136(11) . ?
O122 C122 1.123(12) . ?
O123 C123 1.150(11) . ?
C2 C3 1.406(12) . ?
C3 C4 1.460(12) . ?
C4 C5 1.395(12) . ?
C4 H4 1.0000 . ?
C2A C3A 1.398(12) . ?
C3A C4A 1.470(12) . ?
C4A C5A 1.409(12) . ?
C4A H4A 1.0000 . ?

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
C11 Os1 C12 90.6(4) . . ?
C11 Os1 C10 93.8(4) . . ?
C12 Os1 C10 97.2(4) . . ?
C11 Os1 C3 94.6(4) . . ?
C12 Os1 C3 92.1(3) . . ?
C10 Os1 C3 167.4(4) . . ?
C11 Os1 Os3 100.7(3) . . ?
C12 Os1 Os3 141.8(3) . . ?
C10 Os1 Os3 117.9(3) . . ?
C3 Os1 Os3 51.1(2) . . ?
C11 Os1 Os2 155.5(3) . . ?
C12 Os1 Os2 104.4(3) . . ?
C10 Os1 Os2 103.1(3) . . ?
C3 Os1 Os2 66.1(2) . . ?
Os3 Os1 Os2 55.748(11) . . ?
C11 Os1 H1 173.7(9) . . ?
C12 Os1 H1 85(2) . . ?
C10 Os1 H1 82(2) . . ?
C3 Os1 H1 90.0(19) . . ?
Os3 Os1 H1 85.5(11) . . ?
Os2 Os1 H1 30.7(9) . . ?
C11 Os1 H2 90(4) . . ?
C12 Os1 H2 179(3) . . ?
C10 Os1 H2 83.1(17) . . ?
C3 Os1 H2 87.5(12) . . ?
Os3 Os1 H2 37.6(8) . . ?
Os2 Os1 H2 75(3) . . ?
H1 Os1 H2 94(5) . . ?
C22 Os2 C21 97.4(4) . . ?
C22 Os2 C20 92.6(4) . . ?
C21 Os2 C20 98.4(4) . . ?
C22 Os2 C2 92.9(4) . . ?
C21 Os2 C2 103.2(4) . . ?
C20 Os2 C2 156.7(4) . . ?
C22 Os2 Os3 92.8(3) . . ?
C21 Os2 Os3 158.5(3) . . ?
C20 Os2 Os3 99.9(2) . . ?
C2 Os2 Os3 57.2(2) . . ?
C22 Os2 Os1 149.7(3) . . ?
C21 Os2 Os1 108.0(3) . . ?
C20 Os2 Os1 99.6(3) . . ?
C2 Os2 Os1 65.8(2) . . ?
Os3 Os2 Os1 57.929(11) . . ?
C22 Os2 H1 179.3(13) . . ?
C21 Os2 H1 82.0(17) . . ?
C20 Os2 H1 87(3) . . ?
C2 Os2 H1 87(2) . . ?
Os3 Os2 H1 87.9(11) . . ?
Os1 Os2 H1 31.0(9) . . ?
C30 Os3 C32 92.1(4) . . ?
C30 Os3 C31 101.3(4) . . ?
C32 Os3 C31 93.8(4) . . ?
C30 Os3 C3 160.7(3) . . ?
C32 Os3 C3 101.7(4) . . ?
C31 Os3 C3 91.2(4) . . ?
C30 Os3 C2 137.0(3) . . ?
C32 Os3 C2 82.3(3) . . ?
C31 Os3 C2 121.6(3) . . ?
C3 Os3 C2 35.1(3) . . ?
C30 Os3 Os2 94.0(3) . . ?
C32 Os3 Os2 97.6(3) . . ?
C31 Os3 Os2 160.5(3) . . ?
C3 Os3 Os2 71.1(2) . . ?
C2 Os3 Os2 45.4(2) . . ?
C30 Os3 Os1 115.5(3) . . ?
C32 Os3 Os1 148.1(3) . . ?
C31 Os3 Os1 96.0(3) . . ?
C3 Os3 Os1 47.9(2) . . ?
C2 Os3 Os1 66.76(19) . . ?
Os2 Os3 Os1 66.323(12) . . ?
C30 Os3 H2 81.8(19) . . ?
C32 Os3 H2 173.8(17) . . ?
C31 Os3 H2 87(4) . . ?
C3 Os3 H2 84.3(12) . . ?
C2 Os3 H2 102.5(15) . . ?
Os2 Os3 H2 83(4) . . ?
Os1 Os3 H2 37.6(8) . . ?
C42 Os4 C41 91.2(4) . . ?
C42 Os4 C40 92.0(4) . . ?
C41 Os4 C40 98.0(4) . . ?
C42 Os4 C5 158.3(4) . . ?
C41 Os4 C5 110.2(3) . . ?
C40 Os4 C5 88.1(3) . . ?
C42 Os4 C4 168.4(3) . . ?
C41 Os4 C4 77.2(3) . . ?
C40 Os4 C4 88.8(3) . . ?
C5 Os4 C4 33.3(3) . . ?
C42 Os4 Os5 114.7(3) . . ?
C41 Os4 Os5 138.2(3) . . ?
C40 Os4 Os5 112.3(3) . . ?
C5 Os4 Os5 46.3(2) . . ?
C4 Os4 Os5 75.47(19) . . ?
C42 Os4 Os6 91.9(3) . . ?
C41 Os4 Os6 89.4(3) . . ?
C40 Os4 Os6 171.5(3) . . ?
C5 Os4 Os6 85.4(2) . . ?
C4 Os4 Os6 88.83(19) . . ?
Os5 Os4 Os6 59.230(11) . . ?
C42 Os4 H5 111.9 . . ?
C41 Os4 H5 60.6 . . ?
C40 Os4 H5 147.0 . . ?
C5 Os4 H5 77.8 . . ?
C4 Os4 H5 63.2 . . ?
Os5 Os4 H5 78.9 . . ?
Os6 Os4 H5 36.0 . . ?
C52 Os5 C51 98.3(4) . . ?
C52 Os5 C50 92.0(4) . . ?
C51 Os5 C50 91.3(4) . . ?
C52 Os5 C5 94.8(4) . . ?
C51 Os5 C5 90.0(4) . . ?
C50 Os5 C5 172.8(4) . . ?
C52 Os5 Os6 88.7(3) . . ?
C51 Os5 Os6 172.7(3) . . ?
C50 Os5 Os6 86.6(3) . . ?
C5 Os5 Os6 91.2(2) . . ?
C52 Os5 Os4 131.9(3) . . ?
C51 Os5 Os4 114.8(3) . . ?
C50 Os5 Os4 119.4(3) . . ?
C5 Os5 Os4 53.8(2) . . ?
Os6 Os5 Os4 60.680(11) . . ?
C62 Os6 C61 101.5(4) . . ?
C62 Os6 C63 91.5(4) . . ?
C61 Os6 C63 97.1(4) . . ?
C62 Os6 C60 89.5(4) . . ?
C61 Os6 C60 90.7(4) . . ?
C63 Os6 C60 171.7(4) . . ?
C62 Os6 Os5 94.0(3) . . ?
C61 Os6 Os5 164.4(3) . . ?
C63 Os6 Os5 83.4(3) . . ?
C60 Os6 Os5 88.4(2) . . ?
C62 Os6 Os4 153.4(3) . . ?
C61 Os6 Os4 104.6(3) . . ?
C63 Os6 Os4 80.4(3) . . ?
C60 Os6 Os4 95.2(2) . . ?
Os5 Os6 Os4 60.090(12) . . ?
C62 Os6 H5 153.1 . . ?
C61 Os6 H5 85.8 . . ?
C63 Os6 H5 113.5 . . ?
C60 Os6 H5 64.3 . . ?
Os5 Os6 H5 79.8 . . ?
Os4 Os6 H5 36.3 . . ?
H2A Os7 C71 175(3) . . ?
H2A Os7 C72 92(3) . . ?
C71 Os7 C72 92.2(4) . . ?
H2A Os7 C70 83.0(13) . . ?
C71 Os7 C70 94.7(4) . . ?
C72 Os7 C70 94.1(4) . . ?
H2A Os7 C3A 88.1(10) . . ?
C71 Os7 C3A 93.6(4) . . ?
C72 Os7 C3A 94.2(4) . . ?
C70 Os7 C3A 168.0(4) . . ?
H2A Os7 Os9 37.6(8) . . ?
C71 Os7 Os9 143.1(3) . . ?
C72 Os7 Os9 99.6(2) . . ?
C70 Os7 Os9 118.9(3) . . ?
C3A Os7 Os9 51.1(2) . . ?
H2A Os7 Os8 72(3) . . ?
C71 Os7 Os8 104.3(3) . . ?
C72 Os7 Os8 154.4(2) . . ?
C70 Os7 Os8 103.7(3) . . ?
C3A Os7 Os8 65.7(2) . . ?
Os9 Os7 Os8 55.669(11) . . ?
H2A Os7 H1A 93(4) . . ?
C71 Os7 H1A 83(2) . . ?
C72 Os7 H1A 174.3(11) . . ?
C70 Os7 H1A 83(3) . . ?
C3A Os7 H1A 89(2) . . ?
Os9 Os7 H1A 86.1(11) . . ?
Os8 Os7 H1A 31.1(9) . . ?
H2A Os7 H2A 0(7) . . ?
C71 Os7 H2A 175(3) . . ?
C72 Os7 H2A 92(3) . . ?
C70 Os7 H2A 83.0(13) . . ?
C3A Os7 H2A 88.1(10) . . ?
Os9 Os7 H2A 37.6(8) . . ?
Os8 Os7 H2A 72(3) . . ?
H1A Os7 H2A 93(4) . . ?
C81 Os8 C82 96.5(4) . . ?
C81 Os8 C80 98.6(4) . . ?
C82 Os8 C80 93.5(4) . . ?
C81 Os8 C2A 99.8(4) . . ?
C82 Os8 C2A 93.3(3) . . ?
C80 Os8 C2A 159.5(4) . . ?
C81 Os8 Os9 156.2(3) . . ?
C82 Os8 Os9 92.1(3) . . ?
C80 Os8 Os9 103.0(3) . . ?
C2A Os8 Os9 57.4(2) . . ?
C81 Os8 Os7 108.8(3) . . ?
C82 Os8 Os7 149.4(3) . . ?
C80 Os8 Os7 99.4(3) . . ?
C2A Os8 Os7 66.0(2) . . ?
Os9 Os8 Os7 58.018(11) . . ?
C81 Os8 H1A 83(2) . . ?
C82 Os8 H1A 179.5(9) . . ?
C80 Os8 H1A 86(3) . . ?
C2A Os8 H1A 87(2) . . ?
Os9 Os8 H1A 88.4(11) . . ?
Os7 Os8 H1A 31.2(9) . . ?
C91 Os9 C90 92.4(4) . . ?
C91 Os9 C92 94.1(4) . . ?
C90 Os9 C92 101.9(4) . . ?
C91 Os9 C3A 102.3(4) . . ?
C90 Os9 C3A 159.3(3) . . ?
C92 Os9 C3A 91.6(3) . . ?
C91 Os9 C2A 81.7(3) . . ?
C90 Os9 C2A 137.0(3) . . ?
C92 Os9 C2A 121.0(3) . . ?
C3A Os9 C2A 34.8(3) . . ?
C91 Os9 Os8 97.2(3) . . ?
C90 Os9 Os8 93.4(3) . . ?
C92 Os9 Os8 160.6(3) . . ?
C3A Os9 Os8 70.6(2) . . ?
C2A Os9 Os8 46.00(19) . . ?
C91 Os9 Os7 147.9(3) . . ?
C90 Os9 Os7 114.9(3) . . ?
C92 Os9 Os7 96.1(2) . . ?
C3A Os9 Os7 47.2(2) . . ?
C2A Os9 Os7 67.04(19) . . ?
Os8 Os9 Os7 66.312(12) . . ?
C91 Os9 H2A 172(2) . . ?
C90 Os9 H2A 80.0(15) . . ?
C92 Os9 H2A 90(3) . . ?
C3A Os9 H2A 84.4(9) . . ?
C2A Os9 H2A 102.1(15) . . ?
Os8 Os9 H2A 81(3) . . ?
Os7 Os9 H2A 37.7(8) . . ?
C102 Os10 C101 91.2(4) . . ?
C102 Os10 C100 99.0(4) . . ?
C101 Os10 C100 91.6(4) . . ?
C102 Os10 C5A 111.1(3) . . ?
C101 Os10 C5A 157.2(3) . . ?
C100 Os10 C5A 89.2(3) . . ?
C102 Os10 C4A 78.0(3) . . ?
C101 Os10 C4A 169.2(3) . . ?
C100 Os10 C4A 88.8(3) . . ?
C5A Os10 C4A 33.5(3) . . ?
C102 Os10 Os11 136.7(3) . . ?
C101 Os10 Os11 113.8(3) . . ?
C100 Os10 Os11 114.1(3) . . ?
C5A Os10 Os11 46.2(2) . . ?
C4A Os10 Os11 75.7(2) . . ?
C102 Os10 Os12 86.3(3) . . ?
C101 Os10 Os12 92.7(3) . . ?
C100 Os10 Os12 173.1(3) . . ?
C5A Os10 Os12 84.8(2) . . ?
C4A Os10 Os12 87.94(19) . . ?
Os11 Os10 Os12 59.197(11) . . ?
C102 Os10 H5A 80.5 . . ?
C101 Os10 H5A 56.9 . . ?
C100 Os10 H5A 148.4 . . ?
C5A Os10 H5A 120.8 . . ?
C4A Os10 H5A 121.4 . . ?
Os11 Os10 H5A 84.7 . . ?
Os12 Os10 H5A 36.7 . . ?
C112 Os11 C110 96.8(4) . . ?
C112 Os11 C111 92.6(4) . . ?
C110 Os11 C111 92.1(4) . . ?
C112 Os11 C5A 94.8(3) . . ?
C110 Os11 C5A 90.0(3) . . ?
C111 Os11 C5A 172.1(3) . . ?
C112 Os11 Os12 89.9(3) . . ?
C110 Os11 Os12 173.2(3) . . ?
C111 Os11 Os12 86.5(2) . . ?
C5A Os11 Os12 90.6(2) . . ?
C112 Os11 Os10 133.1(2) . . ?
C110 Os11 Os10 114.4(3) . . ?
C111 Os11 Os10 118.7(2) . . ?
C5A Os11 Os10 53.7(2) . . ?
Os12 Os11 Os10 60.849(11) . . ?
C121 Os12 C122 102.9(4) . . ?
C121 Os12 C123 88.9(4) . . ?
C122 Os12 C123 92.0(4) . . ?
C121 Os12 C120 90.6(4) . . ?
C122 Os12 C120 95.7(4) . . ?
C123 Os12 C120 172.2(4) . . ?
C121 Os12 Os11 92.7(3) . . ?
C122 Os12 Os11 164.4(3) . . ?
C123 Os12 Os11 87.2(3) . . ?
C120 Os12 Os11 85.1(3) . . ?
C121 Os12 Os10 151.9(3) . . ?
C122 Os12 Os10 104.7(3) . . ?
C123 Os12 Os10 95.6(2) . . ?
C120 Os12 Os10 81.3(3) . . ?
Os11 Os12 Os10 59.954(12) . . ?
C121 Os12 H5A 146.1 . . ?
C122 Os12 H5A 83.5 . . ?
C123 Os12 H5A 124.6 . . ?
C120 Os12 H5A 55.5 . . ?
Os11 Os12 H5A 84.2 . . ?
Os10 Os12 H5A 35.1 . . ?
C2 O5 C5 109.6(6) . . ?
C2A O5A C5A 109.3(6) . . ?
O5 C2 C3 108.7(7) . . ?
O5 C2 Os2 133.7(6) . . ?
C3 C2 Os2 117.5(6) . . ?
O5 C2 Os3 119.8(5) . . ?
C3 C2 Os3 66.5(5) . . ?
Os2 C2 Os3 77.3(3) . . ?
C2 C3 C4 106.5(8) . . ?
C2 C3 Os1 108.6(6) . . ?
C4 C3 Os1 143.0(6) . . ?
C2 C3 Os3 78.4(5) . . ?
C4 C3 Os3 117.3(6) . . ?
Os1 C3 Os3 81.1(3) . . ?
C5 C4 C3 108.5(7) . . ?
C5 C4 Os4 67.4(5) . . ?
C3 C4 Os4 120.5(6) . . ?
C5 C4 H4 116.7 . . ?
C3 C4 H4 116.7 . . ?
Os4 C4 H4 116.7 . . ?
C4 C5 O5 106.7(7) . . ?
C4 C5 Os5 139.9(6) . . ?
O5 C5 Os5 113.2(6) . . ?
C4 C5 Os4 79.3(5) . . ?
O5 C5 Os4 115.5(5) . . ?
Os5 C5 Os4 79.9(3) . . ?
O5A C2A C3A 111.3(7) . . ?
O5A C2A Os8 133.5(6) . . ?
C3A C2A Os8 115.1(6) . . ?
O5A C2A Os9 120.9(5) . . ?
C3A C2A Os9 66.2(5) . . ?
Os8 C2A Os9 76.6(3) . . ?
C2A C3A C4A 104.5(7) . . ?
C2A C3A Os7 111.2(6) . . ?
C4A C3A Os7 142.4(6) . . ?
C2A C3A Os9 79.0(5) . . ?
C4A C3A Os9 117.5(6) . . ?
Os7 C3A Os9 81.7(3) . . ?
C5A C4A C3A 108.9(7) . . ?
C5A C4A Os10 66.5(5) . . ?
C3A C4A Os10 121.2(6) . . ?
C5A C4A H4A 116.5 . . ?
C3A C4A H4A 116.5 . . ?
Os10 C4A H4A 116.5 . . ?
C4A C5A O5A 106.0(7) . . ?
C4A C5A Os11 140.3(6) . . ?
O5A C5A Os11 113.6(5) . . ?
C4A C5A Os10 80.0(5) . . ?
O5A C5A Os10 116.3(5) . . ?
Os11 C5A Os10 80.1(3) . . ?
O10 C10 Os1 176.7(9) . . ?
O11 C11 Os1 178.1(8) . . ?
O12 C12 Os1 176.2(8) . . ?
O20 C20 Os2 177.4(8) . . ?
O21 C21 Os2 177.1(8) . . ?
O22 C22 Os2 178.2(8) . . ?
O30 C30 Os3 177.2(8) . . ?
O31 C31 Os3 175.1(9) . . ?
O32 C32 Os3 178.5(8) . . ?
O40 C40 Os4 175.9(8) . . ?
O41 C41 Os4 178.8(8) . . ?
O42 C42 Os4 176.2(8) . . ?
O50 C50 Os5 179.0(8) . . ?
O51 C51 Os5 175.7(9) . . ?
O52 C52 Os5 177.2(8) . . ?
O60 C60 Os6 175.2(8) . . ?
O61 C61 Os6 175.5(8) . . ?
O62 C62 Os6 176.0(8) . . ?
O63 C63 Os6 177.2(8) . . ?
O70 C70 Os7 178.3(8) . . ?
O71 C71 Os7 177.9(9) . . ?
O72 C72 Os7 179.6(8) . . ?
O80 C80 Os8 176.5(9) . . ?
O81 C81 Os8 177.1(8) . . ?
O82 C82 Os8 179.3(9) . . ?
O90 C90 Os9 177.7(8) . . ?
O91 C91 Os9 178.6(8) . . ?
O92 C92 Os9 175.8(8) . . ?
O100 C100 Os10 175.6(8) . . ?
O101 C101 Os10 178.0(8) . . ?
O102 C102 Os10 179.8(9) . . ?
O110 C110 Os11 175.8(8) . . ?
O111 C111 Os11 179.0(8) . . ?
O112 C112 Os11 176.8(8) . . ?
O120 C120 Os12 178.2(8) . . ?
O121 C121 Os12 176.2(8) . . ?
O122 C122 Os12 176.9(9) . . ?
O123 C123 Os12 174.7(8) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.63
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.483
_refine_diff_density_min         -2.436
_refine_diff_density_rms         0.317
####################################################################### 
# 
# 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_p-1
_audit_block_doi                 10.5517/ccdc.csd.cc1z50sy
_database_code_depnum_ccdc_archive 'CCDC 1822080'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8CC01532E 2018
_audit_update_record             
;
2018-02-03 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H4 O18 Os6'
_chemical_formula_weight         1685.44

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.4304(5)
_cell_length_b                   9.4911(5)
_cell_length_c                   20.1170(9)
_cell_angle_alpha                98.507(2)
_cell_angle_beta                 95.159(2)
_cell_angle_gamma                119.2940(10)
_cell_volume                     1525.29(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9901
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      29.97

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1460
_exptl_absorpt_coefficient_mu    24.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1723
_exptl_absorpt_correction_T_max  0.3576
_exptl_absorpt_process_details   '(SADABS, Bruker, 2016)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            61060
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         30.10
_reflns_number_total             8941
_reflns_number_gt                7153
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0118P)²+4.3756P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8941
_refine_ls_number_parameters     422
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0474
_refine_ls_wR_factor_gt          0.0434
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.00473(3) -0.25060(3) 0.135111(12) 0.00981(5) Uani 1 1 d D . .
Os2 Os 0.32697(3) -0.16693(3) 0.186147(12) 0.01014(5) Uani 1 1 d . . .
Os3 Os 0.27324(3) 0.01651(3) 0.092820(11) 0.00962(5) Uani 1 1 d D . .
Os4 Os 0.46644(3) 0.30888(3) 0.324649(11) 0.00939(5) Uani 1 1 d . . .
Os5 Os 0.36864(3) 0.09841(3) 0.416024(12) 0.01043(5) Uani 1 1 d . . .
Os6 Os 0.13608(3) 0.17957(3) 0.354774(12) 0.01038(5) Uani 1 1 d . . .
O10 O -0.1237(5) -0.3694(5) 0.2615(2) 0.0218(10) Uani 1 1 d . . .
O11 O -0.1260(6) -0.5973(5) 0.0452(2) 0.0263(11) Uani 1 1 d . . .
O12 O -0.2972(6) -0.2251(6) 0.0881(3) 0.0305(12) Uani 1 1 d . . .
O20 O 0.6900(5) -0.0531(5) 0.2356(2) 0.0226(10) Uani 1 1 d . . .
O21 O 0.2204(6) -0.3593(6) 0.2986(2) 0.0261(11) Uani 1 1 d . . .
O22 O 0.2841(6) -0.4664(6) 0.0870(2) 0.0268(11) Uani 1 1 d . . .
O30 O 0.0736(5) 0.1807(5) 0.0625(2) 0.0212(10) Uani 1 1 d . . .
O31 O 0.6070(5) 0.3358(6) 0.1389(2) 0.0276(12) Uani 1 1 d . . .
O32 O 0.3253(5) -0.0540(5) -0.0554(2) 0.0191(10) Uani 1 1 d . . .
O40 O 0.4737(6) 0.5215(6) 0.2232(2) 0.0268(11) Uani 1 1 d . . .
O41 O 0.7056(5) 0.5862(6) 0.4467(2) 0.0234(11) Uani 1 1 d . . .
O42 O 0.7615(5) 0.2820(5) 0.2897(2) 0.0224(10) Uani 1 1 d . . .
O50 O 0.5779(5) 0.3264(5) 0.5560(2) 0.0223(10) Uani 1 1 d . . .
O51 O 0.6196(6) -0.0009(6) 0.3840(2) 0.0260(11) Uani 1 1 d . . .
O52 O 0.1380(6) -0.2121(6) 0.4634(3) 0.0317(12) Uani 1 1 d . . .
O60 O 0.0145(5) 0.2075(6) 0.2145(2) 0.0223(10) Uani 1 1 d . . .
O61 O 0.0360(6) 0.4144(6) 0.4329(2) 0.0255(11) Uani 1 1 d . . .
O62 O -0.1719(5) -0.1411(6) 0.3639(3) 0.0255(11) Uani 1 1 d . . .
C2 C 0.2005(7) -0.0203(7) 0.1861(3) 0.0125(12) Uani 1 1 d . . .
C3 C 0.2795(7) 0.0368(7) 0.2526(3) 0.0118(12) Uani 1 1 d . . .
C4 C 0.2564(7) 0.0545(7) 0.3184(3) 0.0084(11) Uani 1 1 d . . .
C10 C -0.0762(7) -0.3271(7) 0.2138(3) 0.0160(13) Uani 1 1 d . . .
C11 C -0.0802(7) -0.4694(8) 0.0779(3) 0.0168(13) Uani 1 1 d . . .
C12 C -0.1832(8) -0.2334(8) 0.1056(3) 0.0195(14) Uani 1 1 d . . .
C20 C 0.5586(7) -0.0843(7) 0.2185(3) 0.0159(13) Uani 1 1 d . . .
C21 C 0.2592(7) -0.2866(7) 0.2566(3) 0.0147(13) Uani 1 1 d . . .
C22 C 0.2980(7) -0.3573(8) 0.1241(3) 0.0155(13) Uani 1 1 d . . .
C30 C 0.1518(7) 0.1229(7) 0.0728(3) 0.0132(13) Uani 1 1 d . . .
C31 C 0.4800(8) 0.2192(8) 0.1214(3) 0.0158(13) Uani 1 1 d . . .
C32 C 0.3068(7) -0.0271(7) -0.0019(3) 0.0148(13) Uani 1 1 d . . .
C40 C 0.4735(8) 0.4413(8) 0.2593(3) 0.0164(13) Uani 1 1 d . . .
C41 C 0.6150(8) 0.4855(7) 0.4014(3) 0.0146(13) Uani 1 1 d . . .
C42 C 0.6479(7) 0.2872(7) 0.3022(3) 0.0129(12) Uani 1 1 d . . .
C50 C 0.4991(7) 0.2389(7) 0.5055(3) 0.0135(12) Uani 1 1 d . . .
C51 C 0.5243(8) 0.0348(8) 0.3970(3) 0.0150(13) Uani 1 1 d . . .
C52 C 0.2258(8) -0.0953(8) 0.4469(3) 0.0152(13) Uani 1 1 d . . .
C60 C 0.0516(7) 0.1927(7) 0.2673(3) 0.0146(13) Uani 1 1 d . . .
C61 C 0.0740(7) 0.3284(8) 0.4059(3) 0.0151(13) Uani 1 1 d . . .
C62 C -0.0619(8) -0.0211(8) 0.3598(3) 0.0150(13) Uani 1 1 d . . .
H1 H 0.088(5) -0.183(5) 0.0611(12) 0.05(2) Uiso 1 1 d D . .
H2 H 0.385(8) -0.083(8) 0.114(3) 0.025(18) Uiso 1 1 d . . .
H3 H 0.228(9) 0.186(9) 0.435(4) 0.04(2) Uiso 1 1 d . . .
H4 H 0.317(8) 0.360(8) 0.350(3) 0.04(2) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C10 1.906(7) . ?
Os1 C12 1.908(7) . ?
Os1 C11 1.944(6) . ?
Os1 C2 2.070(6) . ?
Os1 Os2 2.7848(4) . ?
Os1 Os3 2.8821(3) . ?
Os1 H1 1.80(2) . ?
Os2 C21 1.907(6) . ?
Os2 C22 1.920(6) . ?
Os2 C20 1.931(6) . ?
Os2 C2 2.233(6) . ?
Os2 C3 2.432(6) . ?
Os2 Os3 2.9107(3) . ?
Os2 H2 1.76(6) . ?
Os3 H1 1.80(2) . ?
Os3 C31 1.906(6) . ?
Os3 C30 1.914(6) . ?
Os3 C32 1.976(6) . ?
Os3 C2 2.075(6) . ?
Os3 H1 1.80(2) . ?
Os3 H2 1.79(6) . ?
Os4 C42 1.905(6) . ?
Os4 C41 1.924(6) . ?
Os4 C40 1.932(7) . ?
Os4 C4 2.226(5) . ?
Os4 C3 2.420(6) . ?
Os4 Os5 2.7944(3) . ?
Os4 Os6 2.8978(4) . ?
Os4 H4 1.79(7) . ?
Os5 C51 1.889(6) . ?
Os5 C52 1.909(6) . ?
Os5 C50 1.953(6) . ?
Os5 C4 2.026(5) . ?
Os5 Os6 2.8930(3) . ?
Os5 H3 1.92(7) . ?
Os6 C60 1.913(6) . ?
Os6 C62 1.932(6) . ?
Os6 C61 1.971(6) . ?
Os6 C4 2.108(6) . ?
Os6 H3 1.73(7) . ?
Os6 H4 1.75(7) . ?
O10 C10 1.140(7) . ?
O11 C11 1.137(7) . ?
O12 C12 1.144(8) . ?
O20 C20 1.130(7) . ?
O21 C21 1.142(7) . ?
O22 C22 1.125(7) . ?
O30 C30 1.136(7) . ?
O31 C31 1.138(7) . ?
O32 C32 1.119(7) . ?
O40 C40 1.127(7) . ?
O41 C41 1.131(7) . ?
O42 C42 1.144(7) . ?
O50 C50 1.134(7) . ?
O51 C51 1.142(7) . ?
O52 C52 1.134(7) . ?
O60 C60 1.138(7) . ?
O61 C61 1.131(7) . ?
O62 C62 1.126(7) . ?
C2 C3 1.359(8) . ?
C3 C4 1.361(8) . ?

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
C10 Os1 C12 92.6(3) . . ?
C10 Os1 C11 95.7(2) . . ?
C12 Os1 C11 95.5(3) . . ?
C10 Os1 C2 97.2(2) . . ?
C12 Os1 C2 109.9(2) . . ?
C11 Os1 C2 150.8(2) . . ?
C10 Os1 Os2 93.58(18) . . ?
C12 Os1 Os2 161.79(18) . . ?
C11 Os1 Os2 100.93(18) . . ?
C2 Os1 Os2 52.27(16) . . ?
C10 Os1 Os3 142.85(17) . . ?
C12 Os1 Os3 103.99(19) . . ?
C11 Os1 Os3 115.11(18) . . ?
C2 Os1 Os3 46.02(16) . . ?
Os2 Os1 Os3 61.784(9) . . ?
C10 Os1 H1 177(2) . . ?
C12 Os1 H1 90(2) . . ?
C11 Os1 H1 83.1(13) . . ?
C2 Os1 H1 82.8(7) . . ?
Os2 Os1 H1 84.2(18) . . ?
Os3 Os1 H1 36.9(7) . . ?
C21 Os2 C22 92.0(3) . . ?
C21 Os2 C20 93.1(3) . . ?
C22 Os2 C20 93.3(3) . . ?
C21 Os2 C2 106.2(2) . . ?
C22 Os2 C2 133.2(2) . . ?
C20 Os2 C2 127.2(2) . . ?
C21 Os2 C3 86.4(2) . . ?
C22 Os2 C3 163.6(2) . . ?
C20 Os2 C3 103.1(2) . . ?
C2 Os2 C3 33.5(2) . . ?
C21 Os2 Os1 92.44(18) . . ?
C22 Os2 Os1 90.37(18) . . ?
C20 Os2 Os1 173.24(18) . . ?
C2 Os2 Os1 47.17(15) . . ?
C3 Os2 Os1 73.45(13) . . ?
C21 Os2 Os3 149.37(18) . . ?
C22 Os2 Os3 102.03(18) . . ?
C20 Os2 Os3 112.83(18) . . ?
C2 Os2 Os3 45.24(15) . . ?
C3 Os2 Os3 72.54(14) . . ?
Os1 Os2 Os3 60.750(8) . . ?
C21 Os2 H2 172(2) . . ?
C22 Os2 H2 80(2) . . ?
C20 Os2 H2 87(2) . . ?
C2 Os2 H2 80(2) . . ?
C3 Os2 H2 102(2) . . ?
Os1 Os2 H2 88(2) . . ?
Os3 Os2 H2 35(2) . . ?
H1 Os3 C31 174.6(19) . . ?
H1 Os3 C30 90(2) . . ?
C31 Os3 C30 93.9(3) . . ?
H1 Os3 C32 81.5(9) . . ?
C31 Os3 C32 94.3(2) . . ?
C30 Os3 C32 94.9(2) . . ?
H1 Os3 C2 82.7(7) . . ?
C31 Os3 C2 100.9(2) . . ?
C30 Os3 C2 94.5(2) . . ?
C32 Os3 C2 161.5(2) . . ?
H1 Os3 Os1 36.9(7) . . ?
C31 Os3 Os1 146.25(18) . . ?
C30 Os3 Os1 94.73(17) . . ?
C32 Os3 Os1 117.31(16) . . ?
C2 Os3 Os1 45.89(16) . . ?
H1 Os3 Os2 80.5(18) . . ?
C31 Os3 Os2 98.69(19) . . ?
C30 Os3 Os2 143.77(17) . . ?
C32 Os3 Os2 117.62(18) . . ?
C2 Os3 Os2 49.82(16) . . ?
Os1 Os3 Os2 57.465(8) . . ?
H1 Os3 H1 0(3) . . ?
C31 Os3 H1 174.6(19) . . ?
C30 Os3 H1 90(2) . . ?
C32 Os3 H1 81.5(9) . . ?
C2 Os3 H1 82.7(7) . . ?
Os1 Os3 H1 36.9(7) . . ?
Os2 Os3 H1 80.5(18) . . ?
H1 Os3 H2 90(3) . . ?
C31 Os3 H2 86(2) . . ?
C30 Os3 H2 178(2) . . ?
C32 Os3 H2 87(2) . . ?
C2 Os3 H2 84(2) . . ?
Os1 Os3 H2 84.1(19) . . ?
Os2 Os3 H2 35(2) . . ?
H1 Os3 H2 90(3) . . ?
C42 Os4 C41 88.9(2) . . ?
C42 Os4 C40 95.4(3) . . ?
C41 Os4 C40 98.5(3) . . ?
C42 Os4 C4 107.0(2) . . ?
C41 Os4 C4 132.0(2) . . ?
C40 Os4 C4 123.7(2) . . ?
C42 Os4 C3 88.9(2) . . ?
C41 Os4 C3 162.6(2) . . ?
C40 Os4 C3 98.9(2) . . ?
C4 Os4 C3 33.73(19) . . ?
C42 Os4 Os5 98.80(17) . . ?
C41 Os4 Os5 87.66(18) . . ?
C40 Os4 Os5 164.60(18) . . ?
C4 Os4 Os5 45.88(14) . . ?
C3 Os4 Os5 75.66(14) . . ?
C42 Os4 Os6 153.04(17) . . ?
C41 Os4 Os6 106.71(18) . . ?
C40 Os4 Os6 103.56(18) . . ?
C4 Os4 Os6 46.33(14) . . ?
C3 Os4 Os6 69.59(13) . . ?
Os5 Os4 Os6 61.061(8) . . ?
C42 Os4 H4 172(2) . . ?
C41 Os4 H4 84(2) . . ?
C40 Os4 H4 81(2) . . ?
C4 Os4 H4 81(2) . . ?
C3 Os4 H4 99(2) . . ?
Os5 Os4 H4 85(2) . . ?
Os6 Os4 H4 35(2) . . ?
C51 Os5 C52 95.7(3) . . ?
C51 Os5 C50 93.7(3) . . ?
C52 Os5 C50 97.5(3) . . ?
C51 Os5 C4 98.1(2) . . ?
C52 Os5 C4 103.9(2) . . ?
C50 Os5 C4 154.2(2) . . ?
C51 Os5 Os4 90.96(18) . . ?
C52 Os5 Os4 155.86(18) . . ?
C50 Os5 Os4 105.16(17) . . ?
C4 Os5 Os4 52.08(15) . . ?
C51 Os5 Os6 143.54(18) . . ?
C52 Os5 Os6 101.76(18) . . ?
C50 Os5 Os6 115.03(18) . . ?
C4 Os5 Os6 46.76(16) . . ?
Os4 Os5 Os6 61.235(8) . . ?
C51 Os5 H3 174(2) . . ?
C52 Os5 H3 90(2) . . ?
C50 Os5 H3 84(2) . . ?
C4 Os5 H3 82(2) . . ?
Os4 Os5 H3 84(2) . . ?
Os6 Os5 H3 35(2) . . ?
C60 Os6 C62 95.3(3) . . ?
C60 Os6 C61 93.8(2) . . ?
C62 Os6 C61 94.5(2) . . ?
C60 Os6 C4 96.6(2) . . ?
C62 Os6 C4 93.9(2) . . ?
C61 Os6 C4 165.9(2) . . ?
C60 Os6 Os5 139.93(17) . . ?
C62 Os6 Os5 96.34(18) . . ?
C61 Os6 Os5 123.15(17) . . ?
C4 Os6 Os5 44.43(15) . . ?
C60 Os6 Os4 92.01(17) . . ?
C62 Os6 Os4 143.64(17) . . ?
C61 Os6 Os4 120.47(17) . . ?
C4 Os6 Os4 49.79(15) . . ?
Os5 Os6 Os4 57.704(8) . . ?
C60 Os6 H3 175(2) . . ?
C62 Os6 H3 90(2) . . ?
C61 Os6 H3 85(2) . . ?
C4 Os6 H3 84(2) . . ?
Os5 Os6 H3 40(2) . . ?
Os4 Os6 H3 84(2) . . ?
C60 Os6 H4 85(2) . . ?
C62 Os6 H4 179(2) . . ?
C61 Os6 H4 86(2) . . ?
C4 Os6 H4 85(2) . . ?
Os5 Os6 H4 83(2) . . ?
Os4 Os6 H4 36(2) . . ?
H3 Os6 H4 90(3) . . ?
C3 C2 Os1 130.8(4) . . ?
C3 C2 Os3 135.0(4) . . ?
Os1 C2 Os3 88.1(2) . . ?
C3 C2 Os2 81.3(4) . . ?
Os1 C2 Os2 80.6(2) . . ?
Os3 C2 Os2 84.9(2) . . ?
C2 C3 C4 143.9(6) . . ?
C2 C3 Os4 134.5(4) . . ?
C4 C3 Os4 65.3(3) . . ?
C2 C3 Os2 65.2(3) . . ?
C4 C3 Os2 129.4(4) . . ?
Os4 C3 Os2 132.3(2) . . ?
C3 C4 Os5 142.3(4) . . ?
C3 C4 Os6 122.3(4) . . ?
Os5 C4 Os6 88.8(2) . . ?
C3 C4 Os4 81.0(3) . . ?
Os5 C4 Os4 82.04(19) . . ?
Os6 C4 Os4 83.88(19) . . ?
O10 C10 Os1 178.5(5) . . ?
O11 C11 Os1 178.1(6) . . ?
O12 C12 Os1 179.1(6) . . ?
O20 C20 Os2 172.6(5) . . ?
O21 C21 Os2 178.8(6) . . ?
O22 C22 Os2 178.3(6) . . ?
O30 C30 Os3 176.5(5) . . ?
O31 C31 Os3 176.7(6) . . ?
O32 C32 Os3 179.0(5) . . ?
O40 C40 Os4 176.5(6) . . ?
O41 C41 Os4 177.3(6) . . ?
O42 C42 Os4 176.8(5) . . ?
O50 C50 Os5 176.9(5) . . ?
O51 C51 Os5 177.9(5) . . ?
O52 C52 Os5 178.0(6) . . ?
O60 C60 Os6 174.3(5) . . ?
O61 C61 Os6 177.3(5) . . ?
O62 C62 Os6 176.3(6) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        30.10
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.771
_refine_diff_density_min         -2.041
_refine_diff_density_rms         0.370
####################################################################### 
# 
# 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_b5_twin
_audit_block_doi                 10.5517/ccdc.csd.cc1z50tz
_database_code_depnum_ccdc_archive 'CCDC 1822081'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8CC01532E 2018
_audit_update_record             
;
2018-02-03 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H4 O19 Os6'
_chemical_formula_weight         1713.45

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   15.0941(12)
_cell_length_b                   9.2362(7)
_cell_length_c                   23.5146(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.717(2)
_cell_angle_gamma                90.00
_cell_volume                     3184.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5913
_cell_measurement_theta_min      4.756
_cell_measurement_theta_max      56.908

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2976
_exptl_absorpt_coefficient_mu    23.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0867
_exptl_absorpt_correction_T_max  0.6462
_exptl_absorpt_process_details   '(SADABS, Bruker, 2016)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            8057
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         28.50
_reflns_number_total             8057
_reflns_number_gt                6923
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0532P)²+52.3479P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000086(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8057
_refine_ls_number_parameters     439
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.1039
_refine_ls_wR_factor_gt          0.0953
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.54495(3) 0.74971(5) 0.34018(2) 0.01595(12) Uani 1 1 d D . .
Os2 Os 0.65424(3) 0.49257(5) 0.35744(2) 0.01545(11) Uani 1 1 d D . .
Os3 Os 0.46598(3) 0.47859(6) 0.36521(2) 0.01671(12) Uani 1 1 d D . .
Os4 Os 0.30943(3) 0.34300(5) 0.08992(2) 0.01603(12) Uani 1 1 d . . .
Os5 Os 0.50294(3) 0.35665(5) 0.12026(2) 0.01520(11) Uani 1 1 d D . .
Os6 Os 0.40291(3) 0.61319(5) 0.10432(2) 0.01564(11) Uani 1 1 d D . .
O10 O 0.5988(8) 0.9974(12) 0.4294(5) 0.032(3) Uani 1 1 d . . .
O11 O 0.6375(7) 0.8624(11) 0.2471(5) 0.027(2) Uani 1 1 d . . .
O12 O 0.3647(8) 0.8859(12) 0.2751(6) 0.037(3) Uani 1 1 d . . .
O20 O 0.8144(7) 0.4666(11) 0.4663(5) 0.027(2) Uani 1 1 d . . .
O21 O 0.7774(8) 0.6100(11) 0.2827(5) 0.029(2) Uani 1 1 d . . .
O22 O 0.6625(8) 0.1749(11) 0.3222(5) 0.030(3) Uani 1 1 d . . .
O30 O 0.2747(7) 0.5663(11) 0.2969(5) 0.024(2) Uani 1 1 d . . .
O31 O 0.4426(7) 0.1645(11) 0.3275(5) 0.029(2) Uani 1 1 d . . .
O32 O 0.4058(8) 0.4141(17) 0.4796(5) 0.046(4) Uani 1 1 d . . .
O40 O 0.3248(8) 0.3678(11) -0.0388(5) 0.028(2) Uani 1 1 d . . .
O41 O 0.1122(8) 0.4501(16) 0.0660(6) 0.043(3) Uani 1 1 d . . .
O42 O 0.2936(8) 0.0121(11) 0.0888(5) 0.032(3) Uani 1 1 d . . .
O50 O 0.7072(7) 0.4191(11) 0.1478(5) 0.029(3) Uani 1 1 d . . .
O51 O 0.5085(8) 0.1601(11) 0.0173(4) 0.025(2) Uani 1 1 d . . .
O52 O 0.3286(7) 0.3405(12) 0.2232(5) 0.027(2) Uani 1 1 d . . .
O53 O 0.5050(8) 0.1093(11) 0.2056(5) 0.030(3) Uani 1 1 d . . .
O60 O 0.5303(9) 0.8777(11) 0.1179(5) 0.032(3) Uani 1 1 d . . .
O61 O 0.2925(7) 0.7054(11) -0.0169(4) 0.025(2) Uani 1 1 d . . .
O62 O 0.2593(8) 0.7354(11) 0.1615(5) 0.033(3) Uani 1 1 d . . .
C1 C 0.5273(8) 0.5449(15) 0.2975(6) 0.016(3) Uani 1 1 d . . .
C2 C 0.5043(9) 0.5284(14) 0.2370(6) 0.019(3) Uani 1 1 d . . .
C3 C 0.4814(9) 0.5182(13) 0.1835(6) 0.015(2) Uani 1 1 d . . .
C10 C 0.5777(10) 0.9035(16) 0.3965(7) 0.024(3) Uani 1 1 d . . .
C11 C 0.6044(10) 0.8294(15) 0.2824(6) 0.021(3) Uani 1 1 d . . .
C12 C 0.4333(11) 0.8366(15) 0.2990(8) 0.028(3) Uani 1 1 d . . .
C20 C 0.7550(11) 0.4735(15) 0.4274(7) 0.024(3) Uani 1 1 d . . .
C21 C 0.7328(11) 0.5624(15) 0.3095(7) 0.023(3) Uani 1 1 d . . .
C22 C 0.6618(10) 0.2930(16) 0.3360(8) 0.028(3) Uani 1 1 d . . .
C30 C 0.3462(9) 0.5315(13) 0.3226(6) 0.019(3) Uani 1 1 d . . .
C31 C 0.4491(9) 0.2823(13) 0.3415(6) 0.016(3) Uani 1 1 d . . .
C32 C 0.4303(12) 0.439(2) 0.4377(8) 0.034(4) Uani 1 1 d . . .
C40 C 0.3188(9) 0.3591(14) 0.0078(7) 0.019(3) Uani 1 1 d . . .
C41 C 0.1862(10) 0.4121(16) 0.0739(8) 0.027(3) Uani 1 1 d . . .
C42 C 0.2988(9) 0.1376(14) 0.0884(6) 0.016(3) Uani 1 1 d . . .
C43 C 0.3226(9) 0.3444(15) 0.1748(6) 0.018(3) Uani 1 1 d . . .
C50 C 0.6314(8) 0.4003(15) 0.1375(7) 0.019(3) Uani 1 1 d . . .
C51 C 0.5064(9) 0.2311(15) 0.0557(7) 0.022(3) Uani 1 1 d . . .
C52 C 0.5066(10) 0.1977(15) 0.1731(6) 0.021(3) Uani 1 1 d U . .
C60 C 0.4856(11) 0.7808(16) 0.1148(6) 0.025(3) Uani 1 1 d . . .
C61 C 0.3333(11) 0.6677(15) 0.0289(7) 0.024(3) Uani 1 1 d . . .
C62 C 0.3143(10) 0.6920(15) 0.1413(7) 0.025(3) Uani 1 1 d . . .
H1 H 0.484(10) 0.665(7) 0.389(6) 0.030 Uiso 1 1 d D . .
H2 H 0.582(3) 0.453(17) 0.407(5) 0.030 Uiso 1 1 d D . .
H3 H 0.641(8) 0.666(9) 0.390(4) 0.05(6) Uiso 1 1 d D . .
H4 H 0.488(11) 0.519(11) 0.073(9) 0.054 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C12 1.909(17) . ?
Os1 C10 1.925(15) . ?
Os1 C11 1.941(15) . ?
Os1 C1 2.129(14) . ?
Os1 Os2 2.8652(7) . ?
Os1 Os3 2.8932(7) . ?
Os1 H1 1.81(7) . ?
Os1 H3 1.80(2) . ?
Os2 C22 1.921(15) . ?
Os2 C21 1.931(16) . ?
Os2 C20 1.966(16) . ?
Os2 C1 2.148(12) . ?
Os2 Os3 2.8934(7) . ?
Os2 H2 1.81(7) . ?
Os2 H3 1.80(2) . ?
Os3 C31 1.896(12) . ?
Os3 C30 1.911(14) . ?
Os3 C32 1.940(17) . ?
Os3 C1 2.114(13) . ?
Os3 H1 1.81(7) . ?
Os3 H2 1.81(7) . ?
Os4 C42 1.904(13) . ?
Os4 C41 1.917(15) . ?
Os4 C43 1.958(14) . ?
Os4 C40 1.974(15) . ?
Os4 Os5 2.8404(7) . ?
Os4 Os6 2.8472(7) . ?
Os5 C52 1.915(15) . ?
Os5 C51 1.920(15) . ?
Os5 C50 1.927(12) . ?
Os5 C3 2.186(13) . ?
Os5 Os6 2.7868(7) . ?
Os5 H4 1.85(13) . ?
Os6 C61 1.902(16) . ?
Os6 C62 1.904(15) . ?
Os6 C60 1.966(15) . ?
Os6 C3 2.144(13) . ?
Os6 H4 1.85(13) . ?
O10 C10 1.155(18) . ?
O11 C11 1.109(18) . ?
O12 C12 1.149(19) . ?
O20 C20 1.120(18) . ?
O21 C21 1.114(18) . ?
O22 C22 1.139(18) . ?
O30 C30 1.150(17) . ?
O31 C31 1.134(16) . ?
O32 C32 1.15(2) . ?
O40 C40 1.124(17) . ?
O41 C41 1.144(18) . ?
O42 C42 1.161(16) . ?
O50 C50 1.125(16) . ?
O51 C51 1.122(17) . ?
O52 C43 1.120(17) . ?
O53 C52 1.123(18) . ?
O60 C60 1.113(18) . ?
O61 C61 1.160(19) . ?
O62 C62 1.124(18) . ?
C1 C2 1.390(19) . ?
C2 C3 1.23(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 Os1 C10 95.2(6) . . ?
C12 Os1 C11 89.1(6) . . ?
C10 Os1 C11 96.6(6) . . ?
C12 Os1 C1 97.9(5) . . ?
C10 Os1 C1 164.5(6) . . ?
C11 Os1 C1 91.9(5) . . ?
C12 Os1 Os2 146.0(4) . . ?
C10 Os1 Os2 118.0(5) . . ?
C11 Os1 Os2 93.9(4) . . ?
C1 Os1 Os2 48.2(3) . . ?
C12 Os1 Os3 96.3(4) . . ?
C10 Os1 Os3 123.4(4) . . ?
C11 Os1 Os3 138.7(4) . . ?
C1 Os1 Os3 46.8(4) . . ?
Os2 Os1 Os3 60.324(18) . . ?
C12 Os1 H1 89(5) . . ?
C10 Os1 H1 88(3) . . ?
C11 Os1 H1 175(4) . . ?
C1 Os1 H1 84(3) . . ?
Os2 Os1 H1 85(4) . . ?
Os3 Os1 H1 37(3) . . ?
C12 Os1 H3 170(5) . . ?
C10 Os1 H3 80.7(9) . . ?
C11 Os1 H3 100(6) . . ?
C1 Os1 H3 85.0(12) . . ?
Os2 Os1 H3 37.3(7) . . ?
Os3 Os1 H3 79(5) . . ?
H1 Os1 H3 82(8) . . ?
C22 Os2 C21 94.8(6) . . ?
C22 Os2 C20 92.9(6) . . ?
C21 Os2 C20 93.4(6) . . ?
C22 Os2 C1 98.2(6) . . ?
C21 Os2 C1 96.7(6) . . ?
C20 Os2 C1 164.2(6) . . ?
C22 Os2 Os1 145.7(5) . . ?
C21 Os2 Os1 93.0(4) . . ?
C20 Os2 Os1 119.9(4) . . ?
C1 Os2 Os1 47.6(4) . . ?
C22 Os2 Os3 95.4(5) . . ?
C21 Os2 Os3 143.1(5) . . ?
C20 Os2 Os3 121.3(4) . . ?
C1 Os2 Os3 46.7(4) . . ?
Os1 Os2 Os3 60.318(18) . . ?
C22 Os2 H2 93(5) . . ?
C21 Os2 H2 172(5) . . ?
C20 Os2 H2 85(3) . . ?
C1 Os2 H2 84(3) . . ?
Os1 Os2 H2 81(4) . . ?
Os3 Os2 H2 37(3) . . ?
C22 Os2 H3 169(6) . . ?
C21 Os2 H3 95(6) . . ?
C20 Os2 H3 82.6(8) . . ?
C1 Os2 H3 84.4(12) . . ?
Os1 Os2 H3 37.2(7) . . ?
Os3 Os2 H3 79(5) . . ?
H2 Os2 H3 76(8) . . ?
C31 Os3 C30 92.6(5) . . ?
C31 Os3 C32 91.9(7) . . ?
C30 Os3 C32 94.8(7) . . ?
C31 Os3 C1 96.2(6) . . ?
C30 Os3 C1 93.4(6) . . ?
C32 Os3 C1 168.2(6) . . ?
C31 Os3 Os1 143.2(4) . . ?
C30 Os3 Os1 93.2(4) . . ?
C32 Os3 Os1 123.7(5) . . ?
C1 Os3 Os1 47.2(4) . . ?
C31 Os3 Os2 95.1(4) . . ?
C30 Os3 Os2 141.0(4) . . ?
C32 Os3 Os2 123.0(5) . . ?
C1 Os3 Os2 47.7(3) . . ?
Os1 Os3 Os2 59.358(17) . . ?
C31 Os3 H1 179(5) . . ?
C30 Os3 H1 88(5) . . ?
C32 Os3 H1 88(3) . . ?
C1 Os3 H1 84(3) . . ?
Os1 Os3 H1 37(3) . . ?
Os2 Os3 H1 84(4) . . ?
C31 Os3 H2 95(5) . . ?
C30 Os3 H2 173(5) . . ?
C32 Os3 H2 86(3) . . ?
C1 Os3 H2 85(3) . . ?
Os1 Os3 H2 80(4) . . ?
Os2 Os3 H2 37(3) . . ?
H1 Os3 H2 84(7) . . ?
C42 Os4 C41 104.7(6) . . ?
C42 Os4 C43 90.8(6) . . ?
C41 Os4 C43 93.3(6) . . ?
C42 Os4 C40 94.7(5) . . ?
C41 Os4 C40 94.2(6) . . ?
C43 Os4 C40 169.3(5) . . ?
C42 Os4 Os5 97.3(4) . . ?
C41 Os4 Os5 157.9(4) . . ?
C43 Os4 Os5 83.9(4) . . ?
C40 Os4 Os5 86.2(4) . . ?
C42 Os4 Os6 155.9(4) . . ?
C41 Os4 Os6 99.3(4) . . ?
C43 Os4 Os6 86.9(4) . . ?
C40 Os4 Os6 84.4(4) . . ?
Os5 Os4 Os6 58.677(18) . . ?
C52 Os5 C51 92.7(6) . . ?
C52 Os5 C50 98.7(6) . . ?
C51 Os5 C50 94.4(6) . . ?
C52 Os5 C3 93.9(5) . . ?
C51 Os5 C3 170.6(5) . . ?
C50 Os5 C3 91.1(5) . . ?
C52 Os5 Os6 132.1(4) . . ?
C51 Os5 Os6 121.5(4) . . ?
C50 Os5 Os6 109.7(4) . . ?
C3 Os5 Os6 49.3(3) . . ?
C52 Os5 Os4 89.9(4) . . ?
C51 Os5 Os4 89.7(4) . . ?
C50 Os5 Os4 170.2(4) . . ?
C3 Os5 Os4 83.7(3) . . ?
Os6 Os5 Os4 60.784(18) . . ?
C52 Os5 H4 173(5) . . ?
C51 Os5 H4 92(5) . . ?
C50 Os5 H4 86(6) . . ?
C3 Os5 H4 81(5) . . ?
Os6 Os5 H4 41(5) . . ?
Os4 Os5 H4 85(6) . . ?
C61 Os6 C62 91.8(6) . . ?
C61 Os6 C60 95.9(6) . . ?
C62 Os6 C60 97.8(6) . . ?
C61 Os6 C3 170.9(5) . . ?
C62 Os6 C3 93.6(6) . . ?
C60 Os6 C3 90.6(5) . . ?
C61 Os6 Os5 120.8(4) . . ?
C62 Os6 Os5 132.9(4) . . ?
C60 Os6 Os5 110.2(5) . . ?
C3 Os6 Os5 50.6(3) . . ?
C61 Os6 Os4 88.4(4) . . ?
C62 Os6 Os4 90.4(4) . . ?
C60 Os6 Os4 170.6(5) . . ?
C3 Os6 Os4 84.3(3) . . ?
Os5 Os6 Os4 60.539(18) . . ?
C61 Os6 H4 92(6) . . ?
C62 Os6 H4 174(5) . . ?
C60 Os6 H4 87(6) . . ?
C3 Os6 H4 82(5) . . ?
Os5 Os6 H4 41(5) . . ?
Os4 Os6 H4 85(6) . . ?
C2 C1 Os3 133.8(10) . . ?
C2 C1 Os1 123.6(10) . . ?
Os3 C1 Os1 86.0(5) . . ?
C2 C1 Os2 127.9(10) . . ?
Os3 C1 Os2 85.5(5) . . ?
Os1 C1 Os2 84.1(5) . . ?
C3 C2 C1 177.3(14) . . ?
C2 C3 Os6 145.4(11) . . ?
C2 C3 Os5 134.4(10) . . ?
Os6 C3 Os5 80.1(5) . . ?
O10 C10 Os1 178.1(13) . . ?
O11 C11 Os1 173.4(12) . . ?
O12 C12 Os1 177.9(15) . . ?
O20 C20 Os2 177.1(13) . . ?
O21 C21 Os2 176.3(12) . . ?
O22 C22 Os2 177.1(14) . . ?
O30 C30 Os3 178.6(12) . . ?
O31 C31 Os3 177.2(12) . . ?
O32 C32 Os3 177.4(15) . . ?
O40 C40 Os4 179.4(13) . . ?
O41 C41 Os4 177.4(15) . . ?
O42 C42 Os4 178.4(13) . . ?
O52 C43 Os4 177.5(12) . . ?
O50 C50 Os5 176.8(13) . . ?
O51 C51 Os5 178.6(13) . . ?
O53 C52 Os5 175.6(12) . . ?
O60 C60 Os6 176.4(14) . . ?
O61 C61 Os6 177.6(13) . . ?
O62 C62 Os6 177.2(15) . . ?

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
C12 Os1 Os2 C22 -1.8(13) . . . . ?
C10 Os1 Os2 C22 164.4(10) . . . . ?
C11 Os1 Os2 C22 -96.0(10) . . . . ?
C1 Os1 Os2 C22 -6.8(10) . . . . ?
Os3 Os1 Os2 C22 49.9(9) . . . . ?
C12 Os1 Os2 C21 101.4(10) . . . . ?
C10 Os1 Os2 C21 -92.4(7) . . . . ?
C11 Os1 Os2 C21 7.2(6) . . . . ?
C1 Os1 Os2 C21 96.3(6) . . . . ?
Os3 Os1 Os2 C21 153.1(4) . . . . ?
C12 Os1 Os2 C20 -163.0(10) . . . . ?
C10 Os1 Os2 C20 3.2(7) . . . . ?
C11 Os1 Os2 C20 102.8(6) . . . . ?
C1 Os1 Os2 C20 -168.0(7) . . . . ?
Os3 Os1 Os2 C20 -111.2(5) . . . . ?
C12 Os1 Os2 C1 5.0(10) . . . . ?
C10 Os1 Os2 C1 171.2(7) . . . . ?
C11 Os1 Os2 C1 -89.1(6) . . . . ?
Os3 Os1 Os2 C1 56.8(5) . . . . ?
C12 Os1 Os2 Os3 -51.8(9) . . . . ?
C10 Os1 Os2 Os3 114.4(5) . . . . ?
C11 Os1 Os2 Os3 -145.9(4) . . . . ?
C1 Os1 Os2 Os3 -56.8(5) . . . . ?
C12 Os1 Os3 C31 102.0(8) . . . . ?
C10 Os1 Os3 C31 -157.5(9) . . . . ?
C11 Os1 Os3 C31 6.1(9) . . . . ?
C1 Os1 Os3 C31 7.1(8) . . . . ?
Os2 Os1 Os3 C31 -51.8(7) . . . . ?
C12 Os1 Os3 C30 3.2(6) . . . . ?
C10 Os1 Os3 C30 103.7(7) . . . . ?
C11 Os1 Os3 C30 -92.7(8) . . . . ?
C1 Os1 Os3 C30 -91.7(6) . . . . ?
Os2 Os1 Os3 C30 -150.6(4) . . . . ?
C12 Os1 Os3 C32 -94.7(8) . . . . ?
C10 Os1 Os3 C32 5.8(8) . . . . ?
C11 Os1 Os3 C32 169.4(9) . . . . ?
C1 Os1 Os3 C32 170.4(8) . . . . ?
Os2 Os1 Os3 C32 111.5(6) . . . . ?
C12 Os1 Os3 C1 94.9(7) . . . . ?
C10 Os1 Os3 C1 -164.6(7) . . . . ?
C11 Os1 Os3 C1 -1.0(8) . . . . ?
Os2 Os1 Os3 C1 -58.9(5) . . . . ?
C12 Os1 Os3 Os2 153.8(5) . . . . ?
C10 Os1 Os3 Os2 -105.7(5) . . . . ?
C11 Os1 Os3 Os2 57.9(6) . . . . ?
C1 Os1 Os3 Os2 58.9(5) . . . . ?
C22 Os2 Os3 C31 -2.5(7) . . . . ?
C21 Os2 Os3 C31 103.0(8) . . . . ?
C20 Os2 Os3 C31 -99.3(6) . . . . ?
C1 Os2 Os3 C31 93.7(7) . . . . ?
Os1 Os2 Os3 C31 151.8(4) . . . . ?
C22 Os2 Os3 C30 -103.1(8) . . . . ?
C21 Os2 Os3 C30 2.4(9) . . . . ?
C20 Os2 Os3 C30 160.1(7) . . . . ?
C1 Os2 Os3 C30 -6.9(8) . . . . ?
Os1 Os2 Os3 C30 51.2(6) . . . . ?
C22 Os2 Os3 C32 93.1(8) . . . . ?
C21 Os2 Os3 C32 -161.4(9) . . . . ?
C20 Os2 Os3 C32 -3.7(8) . . . . ?
C1 Os2 Os3 C32 -170.7(8) . . . . ?
Os1 Os2 Os3 C32 -112.6(6) . . . . ?
C22 Os2 Os3 C1 -96.2(7) . . . . ?
C21 Os2 Os3 C1 9.3(8) . . . . ?
C20 Os2 Os3 C1 167.0(7) . . . . ?
Os1 Os2 Os3 C1 58.1(5) . . . . ?
C22 Os2 Os3 Os1 -154.3(5) . . . . ?
C21 Os2 Os3 Os1 -48.8(7) . . . . ?
C20 Os2 Os3 Os1 108.9(5) . . . . ?
C1 Os2 Os3 Os1 -58.1(5) . . . . ?
C42 Os4 Os5 C52 -39.8(5) . . . . ?
C41 Os4 Os5 C52 133.9(14) . . . . ?
C43 Os4 Os5 C52 50.2(5) . . . . ?
C40 Os4 Os5 C52 -134.1(5) . . . . ?
Os6 Os4 Os5 C52 140.3(4) . . . . ?
C42 Os4 Os5 C51 52.9(6) . . . . ?
C41 Os4 Os5 C51 -133.3(14) . . . . ?
C43 Os4 Os5 C51 142.9(6) . . . . ?
C40 Os4 Os5 C51 -41.3(6) . . . . ?
Os6 Os4 Os5 C51 -127.0(4) . . . . ?
C42 Os4 Os5 C50 168(3) . . . . ?
C41 Os4 Os5 C50 -18(3) . . . . ?
C43 Os4 Os5 C50 -102(3) . . . . ?
C40 Os4 Os5 C50 74(3) . . . . ?
Os6 Os4 Os5 C50 -12(3) . . . . ?
C42 Os4 Os5 C3 -133.7(5) . . . . ?
C41 Os4 Os5 C3 40.0(14) . . . . ?
C43 Os4 Os5 C3 -43.7(5) . . . . ?
C40 Os4 Os5 C3 132.0(5) . . . . ?
Os6 Os4 Os5 C3 46.3(3) . . . . ?
C42 Os4 Os5 Os6 180.0(4) . . . . ?
C41 Os4 Os5 Os6 -6.3(13) . . . . ?
C43 Os4 Os5 Os6 -90.0(4) . . . . ?
C40 Os4 Os5 Os6 85.7(4) . . . . ?
C52 Os5 Os6 C61 -127.5(8) . . . . ?
C51 Os5 Os6 C61 1.4(7) . . . . ?
C50 Os5 Os6 C61 109.8(7) . . . . ?
C3 Os5 Os6 C61 -176.5(7) . . . . ?
Os4 Os5 Os6 C61 -68.1(5) . . . . ?
C52 Os5 Os6 C62 -0.4(9) . . . . ?
C51 Os5 Os6 C62 128.6(8) . . . . ?
C50 Os5 Os6 C62 -123.0(8) . . . . ?
C3 Os5 Os6 C62 -49.3(8) . . . . ?
Os4 Os5 Os6 C62 59.1(7) . . . . ?
C52 Os5 Os6 C60 122.2(7) . . . . ?
C51 Os5 Os6 C60 -108.8(6) . . . . ?
C50 Os5 Os6 C60 -0.4(6) . . . . ?
C3 Os5 Os6 C60 73.3(6) . . . . ?
Os4 Os5 Os6 C60 -178.3(4) . . . . ?
C52 Os5 Os6 C3 49.0(7) . . . . ?
C51 Os5 Os6 C3 177.9(6) . . . . ?
C50 Os5 Os6 C3 -73.7(6) . . . . ?
Os4 Os5 Os6 C3 108.4(4) . . . . ?
C52 Os5 Os6 Os4 -59.5(5) . . . . ?
C51 Os5 Os6 Os4 69.5(5) . . . . ?
C50 Os5 Os6 Os4 177.9(5) . . . . ?
C3 Os5 Os6 Os4 -108.4(4) . . . . ?
C42 Os4 Os6 C61 127.1(10) . . . . ?
C41 Os4 Os6 C61 -55.2(7) . . . . ?
C43 Os4 Os6 C61 -148.1(6) . . . . ?
C40 Os4 Os6 C61 38.1(6) . . . . ?
Os5 Os4 Os6 C61 127.2(4) . . . . ?
C42 Os4 Os6 C62 -141.1(11) . . . . ?
C41 Os4 Os6 C62 36.6(7) . . . . ?
C43 Os4 Os6 C62 -56.3(6) . . . . ?
C40 Os4 Os6 C62 130.0(6) . . . . ?
Os5 Os4 Os6 C62 -141.0(5) . . . . ?
C42 Os4 Os6 C60 10(3) . . . . ?
C41 Os4 Os6 C60 -173(3) . . . . ?
C43 Os4 Os6 C60 95(3) . . . . ?
C40 Os4 Os6 C60 -79(3) . . . . ?
Os5 Os4 Os6 C60 10(3) . . . . ?
C42 Os4 Os6 C3 -47.5(10) . . . . ?
C41 Os4 Os6 C3 130.2(6) . . . . ?
C43 Os4 Os6 C3 37.3(5) . . . . ?
C40 Os4 Os6 C3 -136.5(5) . . . . ?
Os5 Os4 Os6 C3 -47.4(3) . . . . ?
C42 Os4 Os6 Os5 -0.1(9) . . . . ?
C41 Os4 Os6 Os5 177.6(5) . . . . ?
C43 Os4 Os6 Os5 84.8(4) . . . . ?
C40 Os4 Os6 Os5 -89.0(4) . . . . ?
C31 Os3 C1 C2 49.7(14) . . . . ?
C30 Os3 C1 C2 -43.3(14) . . . . ?
C32 Os3 C1 C2 -177(3) . . . . ?
Os1 Os3 C1 C2 -134.5(16) . . . . ?
Os2 Os3 C1 C2 141.1(16) . . . . ?
C31 Os3 C1 Os1 -175.7(5) . . . . ?
C30 Os3 C1 Os1 91.2(5) . . . . ?
C32 Os3 C1 Os1 -43(3) . . . . ?
Os2 Os3 C1 Os1 -84.4(4) . . . . ?
C31 Os3 C1 Os2 -91.3(5) . . . . ?
C30 Os3 C1 Os2 175.6(5) . . . . ?
C32 Os3 C1 Os2 42(3) . . . . ?
Os1 Os3 C1 Os2 84.4(4) . . . . ?
C12 Os1 C1 C2 50.5(12) . . . . ?
C10 Os1 C1 C2 -162.4(18) . . . . ?
C11 Os1 C1 C2 -38.8(12) . . . . ?
Os2 Os1 C1 C2 -132.3(13) . . . . ?
Os3 Os1 C1 C2 141.8(13) . . . . ?
C12 Os1 C1 Os3 -91.3(6) . . . . ?
C10 Os1 C1 Os3 56(2) . . . . ?
C11 Os1 C1 Os3 179.3(5) . . . . ?
Os2 Os1 C1 Os3 85.9(4) . . . . ?
C12 Os1 C1 Os2 -177.2(6) . . . . ?
C10 Os1 C1 Os2 -30(2) . . . . ?
C11 Os1 C1 Os2 93.4(5) . . . . ?
Os3 Os1 C1 Os2 -85.9(4) . . . . ?
C22 Os2 C1 C2 -55.2(14) . . . . ?
C21 Os2 C1 C2 40.7(13) . . . . ?
C20 Os2 C1 C2 170.2(17) . . . . ?
Os1 Os2 C1 C2 128.7(14) . . . . ?
Os3 Os2 C1 C2 -144.9(15) . . . . ?
C22 Os2 C1 Os3 89.7(6) . . . . ?
C21 Os2 C1 Os3 -174.4(5) . . . . ?
C20 Os2 C1 Os3 -45(2) . . . . ?
Os1 Os2 C1 Os3 -86.4(5) . . . . ?
C22 Os2 C1 Os1 176.1(6) . . . . ?
C21 Os2 C1 Os1 -88.0(5) . . . . ?
C20 Os2 C1 Os1 41(2) . . . . ?
Os3 Os2 C1 Os1 86.4(5) . . . . ?
Os3 C1 C2 C3 76(33) . . . . ?
Os1 C1 C2 C3 -45(33) . . . . ?
Os2 C1 C2 C3 -157(32) . . . . ?
C1 C2 C3 Os6 11(34) . . . . ?
C1 C2 C3 Os5 -164(32) . . . . ?
C61 Os6 C3 C2 -157(3) . . . . ?
C62 Os6 C3 C2 -30(2) . . . . ?
C60 Os6 C3 C2 68(2) . . . . ?
Os5 Os6 C3 C2 -176(2) . . . . ?
Os4 Os6 C3 C2 -120.0(19) . . . . ?
C61 Os6 C3 Os5 19(4) . . . . ?
C62 Os6 C3 Os5 146.2(5) . . . . ?
C60 Os6 C3 Os5 -116.0(5) . . . . ?
Os4 Os6 C3 Os5 56.1(3) . . . . ?
C52 Os5 C3 C2 31.1(15) . . . . ?
C51 Os5 C3 C2 166(3) . . . . ?
C50 Os5 C3 C2 -67.8(15) . . . . ?
Os6 Os5 C3 C2 176.9(17) . . . . ?
Os4 Os5 C3 C2 120.5(15) . . . . ?
C52 Os5 C3 Os6 -145.9(5) . . . . ?
C51 Os5 C3 Os6 -11(3) . . . . ?
C50 Os5 C3 Os6 115.3(5) . . . . ?
Os4 Os5 C3 Os6 -56.4(3) . . . . ?
C12 Os1 C10 O10 -97(45) . . . . ?
C11 Os1 C10 O10 -7(45) . . . . ?
C1 Os1 C10 O10 116(44) . . . . ?
Os2 Os1 C10 O10 91(45) . . . . ?
Os3 Os1 C10 O10 162(45) . . . . ?
C12 Os1 C11 O11 -101(11) . . . . ?
C10 Os1 C11 O11 164(11) . . . . ?
C1 Os1 C11 O11 -3(11) . . . . ?
Os2 Os1 C11 O11 45(11) . . . . ?
Os3 Os1 C11 O11 -2(12) . . . . ?
C10 Os1 C12 O12 -103(40) . . . . ?
C11 Os1 C12 O12 161(40) . . . . ?
C1 Os1 C12 O12 69(40) . . . . ?
Os2 Os1 C12 O12 65(40) . . . . ?
Os3 Os1 C12 O12 22(40) . . . . ?
C22 Os2 C20 O20 116(27) . . . . ?
C21 Os2 C20 O20 21(27) . . . . ?
C1 Os2 C20 O20 -108(27) . . . . ?
Os1 Os2 C20 O20 -74(27) . . . . ?
Os3 Os2 C20 O20 -145(27) . . . . ?
C22 Os2 C21 O21 178(100) . . . . ?
C20 Os2 C21 O21 -88(22) . . . . ?
C1 Os2 C21 O21 80(22) . . . . ?
Os1 Os2 C21 O21 32(22) . . . . ?
Os3 Os2 C21 O21 73(22) . . . . ?
C21 Os2 C22 O22 -113(31) . . . . ?
C20 Os2 C22 O22 153(31) . . . . ?
C1 Os2 C22 O22 -16(31) . . . . ?
Os1 Os2 C22 O22 -11(32) . . . . ?
Os3 Os2 C22 O22 31(31) . . . . ?
C31 Os3 C30 O30 -157(51) . . . . ?
C32 Os3 C30 O30 111(51) . . . . ?
C1 Os3 C30 O30 -60(51) . . . . ?
Os1 Os3 C30 O30 -13(51) . . . . ?
Os2 Os3 C30 O30 -55(51) . . . . ?
C30 Os3 C31 O31 150(27) . . . . ?
C32 Os3 C31 O31 -115(27) . . . . ?
C1 Os3 C31 O31 56(27) . . . . ?
Os1 Os3 C31 O31 51(28) . . . . ?
Os2 Os3 C31 O31 8(27) . . . . ?
C31 Os3 C32 O32 -62(38) . . . . ?
C30 Os3 C32 O32 31(38) . . . . ?
C1 Os3 C32 O32 165(36) . . . . ?
Os1 Os3 C32 O32 128(38) . . . . ?
Os2 Os3 C32 O32 -160(38) . . . . ?
C42 Os4 C40 O40 -71(100) . . . . ?
C41 Os4 C40 O40 -176(100) . . . . ?
C43 Os4 C40 O40 49(100) . . . . ?
Os5 Os4 C40 O40 26(100) . . . . ?
Os6 Os4 C40 O40 85(100) . . . . ?
C42 Os4 C41 O41 53(36) . . . . ?
C43 Os4 C41 O41 -39(36) . . . . ?
C40 Os4 C41 O41 149(36) . . . . ?
Os5 Os4 C41 O41 -121(36) . . . . ?
Os6 Os4 C41 O41 -126(36) . . . . ?
C41 Os4 C42 O42 -126(47) . . . . ?
C43 Os4 C42 O42 -32(47) . . . . ?
C40 Os4 C42 O42 139(47) . . . . ?
Os5 Os4 C42 O42 52(47) . . . . ?
Os6 Os4 C42 O42 52(48) . . . . ?
C42 Os4 C43 O52 -23(29) . . . . ?
C41 Os4 C43 O52 82(29) . . . . ?
C40 Os4 C43 O52 -144(28) . . . . ?
Os5 Os4 C43 O52 -120(29) . . . . ?
Os6 Os4 C43 O52 -179(100) . . . . ?
C52 Os5 C50 O50 36(24) . . . . ?
C51 Os5 C50 O50 -57(24) . . . . ?
C3 Os5 C50 O50 131(24) . . . . ?
Os6 Os5 C50 O50 177(100) . . . . ?
Os4 Os5 C50 O50 -172(22) . . . . ?
C52 Os5 C51 O51 -178(100) . . . . ?
C50 Os5 C51 O51 -79(52) . . . . ?
C3 Os5 C51 O51 47(53) . . . . ?
Os6 Os5 C51 O51 37(52) . . . . ?
Os4 Os5 C51 O51 92(52) . . . . ?
C51 Os5 C52 O53 -143(17) . . . . ?
C50 Os5 C52 O53 122(17) . . . . ?
C3 Os5 C52 O53 30(17) . . . . ?
Os6 Os5 C52 O53 -5(18) . . . . ?
Os4 Os5 C52 O53 -53(17) . . . . ?
C61 Os6 C60 O60 -5(23) . . . . ?
C62 Os6 C60 O60 -98(23) . . . . ?
C3 Os6 C60 O60 169(23) . . . . ?
Os5 Os6 C60 O60 121(23) . . . . ?
Os4 Os6 C60 O60 112(23) . . . . ?
C62 Os6 C61 O61 91(32) . . . . ?
C60 Os6 C61 O61 -7(32) . . . . ?
C3 Os6 C61 O61 -142(30) . . . . ?
Os5 Os6 C61 O61 -125(32) . . . . ?
Os4 Os6 C61 O61 -179(100) . . . . ?
C61 Os6 C62 O62 50(27) . . . . ?
C60 Os6 C62 O62 147(27) . . . . ?
C3 Os6 C62 O62 -122(27) . . . . ?
Os5 Os6 C62 O62 -86(27) . . . . ?
Os4 Os6 C62 O62 -38(27) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.50
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.348
_refine_diff_density_min         -2.204
_refine_diff_density_rms         0.452
####################################################################### 
# 
# 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_p-1patt
_audit_block_doi                 10.5517/ccdc.csd.cc1zmr4h
_database_code_depnum_ccdc_archive 'CCDC 1836227'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8CC01532E 2018
_audit_update_record             
;
2018-04-11 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        triosmiumnonacarbonyl(furyne)dihydride
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H4 O10 Os3'
_chemical_formula_weight         890.76

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.6127(4)
_cell_length_b                   9.0730(4)
_cell_length_c                   12.9331(6)
_cell_angle_alpha                79.0150(10)
_cell_angle_beta                 79.9380(10)
_cell_angle_gamma                68.3600(10)
_cell_volume                     916.13(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    8147
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      28.28

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_absorpt_coefficient_mu    20.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.164
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10992
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         28.29
_reflns_number_total             4439
_reflns_number_gt                3982
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART V5.632 (Bruker, 2005)'
_computing_cell_refinement       'SAINT+  V6.45 (Bruker, 2003)'
_computing_data_reduction        'SAINT+  V6.45'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0725P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4439
_refine_ls_number_parameters     242
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.1102
_refine_ls_wR_factor_gt          0.1073
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.70007(3) 0.01826(3) 0.76191(2) 0.03571(10) Uani 1 1 d D . .
Os2 Os 0.47256(3) 0.37342(3) 0.73890(3) 0.03907(11) Uani 1 1 d D . .
Os3 Os 0.82874(3) 0.26126(3) 0.68468(2) 0.03760(11) Uani 1 1 d . . .
O1 O 0.8418(9) 0.1118(8) 0.9394(6) 0.0656(18) Uani 1 1 d . . .
O11 O 0.5193(13) -0.1717(12) 0.9237(9) 0.102(3) Uani 1 1 d . . .
O12 O 0.6640(12) -0.0663(10) 0.5502(7) 0.087(3) Uani 1 1 d . . .
O13 O 1.0362(9) -0.2477(8) 0.7849(7) 0.069(2) Uani 1 1 d . . .
O21 O 0.2606(11) 0.3955(10) 0.5628(7) 0.084(2) Uani 1 1 d . . .
O22 O 0.1897(11) 0.3878(12) 0.9194(8) 0.091(3) Uani 1 1 d . . .
O23 O 0.4176(11) 0.7297(8) 0.7122(10) 0.099(3) Uani 1 1 d . . .
O31 O 0.9161(12) 0.1818(10) 0.4593(7) 0.086(2) Uani 1 1 d . . .
O32 O 1.1814(9) 0.0728(10) 0.7465(9) 0.098(3) Uani 1 1 d . . .
O33 O 0.8827(11) 0.5821(8) 0.6539(8) 0.086(3) Uani 1 1 d . . .
C2 C 0.7430(10) 0.1516(9) 0.8592(6) 0.0436(16) Uani 1 1 d . . .
C3 C 0.6584(10) 0.3158(9) 0.8422(7) 0.0440(16) Uani 1 1 d . . .
C4 C 0.7066(12) 0.3835(12) 0.9197(8) 0.059(2) Uani 1 1 d . . .
H4 H 0.6719 0.4906 0.9290 0.070 Uiso 1 1 calc R . .
C5 C 0.8135(16) 0.2552(15) 0.9752(9) 0.073(3) Uani 1 1 d . . .
H5 H 0.8628 0.2627 1.0315 0.088 Uiso 1 1 calc R . .
C11 C 0.5830(12) -0.0994(10) 0.8612(8) 0.056(2) Uani 1 1 d . . .
C12 C 0.6704(12) -0.0393(10) 0.6289(8) 0.053(2) Uani 1 1 d . . .
C13 C 0.9119(10) -0.1478(9) 0.7745(7) 0.0449(17) Uani 1 1 d . . .
C21 C 0.3367(11) 0.3891(11) 0.6293(7) 0.052(2) Uani 1 1 d . . .
C22 C 0.2944(11) 0.3841(11) 0.8526(9) 0.057(2) Uani 1 1 d . . .
C23 C 0.4333(11) 0.5999(10) 0.7237(10) 0.065(3) Uani 1 1 d . . .
C31 C 0.8883(11) 0.2094(10) 0.5442(8) 0.054(2) Uani 1 1 d . . .
C32 C 1.0470(10) 0.1456(10) 0.7228(9) 0.057(2) Uani 1 1 d . . .
C33 C 0.8634(11) 0.4636(10) 0.6647(9) 0.059(2) Uani 1 1 d . . .
H1 H 0.498(4) 0.1673(16) 0.740(9) 0.070 Uiso 1 1 d D . .
H2 H 0.625(8) 0.362(8) 0.609(6) 0.022(16) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C13 1.900(8) . ?
Os1 C11 1.903(9) . ?
Os1 C12 1.973(9) . ?
Os1 C2 2.063(8) . ?
Os1 Os3 2.7682(4) . ?
Os1 Os2 3.0811(4) . ?
Os1 H1 1.800(10) . ?
Os2 C22 1.919(10) . ?
Os2 C23 1.932(9) . ?
Os2 C21 1.944(9) . ?
Os2 C3 2.117(8) . ?
Os2 Os3 2.8558(4) . ?
Os2 H1 1.800(10) . ?
Os2 H2 1.93(7) . ?
Os3 C32 1.884(8) . ?
Os3 C31 1.899(11) . ?
Os3 C33 1.930(8) . ?
Os3 C3 2.313(8) . ?
Os3 C2 2.394(8) . ?
Os3 H2 1.99(7) . ?
O1 C2 1.367(10) . ?
O1 C5 1.387(13) . ?
O11 C11 1.138(11) . ?
O12 C12 1.106(11) . ?
O13 C13 1.129(10) . ?
O21 C21 1.149(11) . ?
O22 C22 1.130(12) . ?
O23 C23 1.118(11) . ?
O31 C31 1.138(12) . ?
O32 C32 1.163(11) . ?
O33 C33 1.127(10) . ?
C2 C3 1.389(10) . ?
C3 C4 1.457(11) . ?
C4 C5 1.357(16) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Os1 C11 93.2(4) . . ?
C13 Os1 C12 93.8(4) . . ?
C11 Os1 C12 99.7(4) . . ?
C13 Os1 C2 93.6(3) . . ?
C11 Os1 C2 100.9(4) . . ?
C12 Os1 C2 157.7(3) . . ?
C13 Os1 Os3 95.8(2) . . ?
C11 Os1 Os3 156.8(3) . . ?
C12 Os1 Os3 101.1(3) . . ?
C2 Os1 Os3 57.2(2) . . ?
C13 Os1 Os2 152.4(2) . . ?
C11 Os1 Os2 108.0(3) . . ?
C12 Os1 Os2 99.7(2) . . ?
C2 Os1 Os2 65.7(2) . . ?
Os3 Os1 Os2 58.155(9) . . ?
C13 Os1 H1 175(3) . . ?
C11 Os1 H1 87(3) . . ?
C12 Os1 H1 81(3) . . ?
C2 Os1 H1 92(2) . . ?
Os3 Os1 H1 86.1(16) . . ?
Os2 Os1 H1 31.1(4) . . ?
C22 Os2 C23 93.2(4) . . ?
C22 Os2 C21 94.7(4) . . ?
C23 Os2 C21 95.7(4) . . ?
C22 Os2 C3 93.6(4) . . ?
C23 Os2 C3 92.7(4) . . ?
C21 Os2 C3 167.8(3) . . ?
C22 Os2 Os3 144.7(3) . . ?
C23 Os2 Os3 98.8(3) . . ?
C21 Os2 Os3 116.8(3) . . ?
C3 Os2 Os3 52.9(2) . . ?
C22 Os2 Os1 104.3(3) . . ?
C23 Os2 Os1 153.0(3) . . ?
C21 Os2 Os1 103.0(3) . . ?
C3 Os2 Os1 66.2(2) . . ?
Os3 Os2 Os1 55.427(8) . . ?
C22 Os2 H1 88(3) . . ?
C23 Os2 H1 174(3) . . ?
C21 Os2 H1 78(2) . . ?
C3 Os2 H1 93.5(18) . . ?
Os3 Os2 H1 83.4(15) . . ?
Os1 Os2 H1 31.1(4) . . ?
C22 Os2 H2 170(2) . . ?
C23 Os2 H2 88.8(19) . . ?
C21 Os2 H2 75(2) . . ?
C3 Os2 H2 96(2) . . ?
Os3 Os2 H2 44(2) . . ?
Os1 Os2 H2 77.5(19) . . ?
H1 Os2 H2 89(4) . . ?
C32 Os3 C31 93.1(4) . . ?
C32 Os3 C33 92.7(4) . . ?
C31 Os3 C33 100.6(4) . . ?
C32 Os3 C3 105.7(4) . . ?
C31 Os3 C3 157.0(3) . . ?
C33 Os3 C3 91.7(4) . . ?
C32 Os3 C2 83.7(4) . . ?
C31 Os3 C2 140.2(3) . . ?
C33 Os3 C2 119.1(4) . . ?
C3 Os3 C2 34.3(3) . . ?
C32 Os3 Os1 96.1(3) . . ?
C31 Os3 Os1 95.0(3) . . ?
C33 Os3 Os1 161.6(3) . . ?
C3 Os3 Os1 70.39(19) . . ?
C2 Os3 Os1 46.40(19) . . ?
C32 Os3 Os2 150.3(3) . . ?
C31 Os3 Os2 111.4(3) . . ?
C33 Os3 Os2 98.6(3) . . ?
C3 Os3 Os2 46.9(2) . . ?
C2 Os3 Os2 66.85(18) . . ?
Os1 Os3 Os2 66.417(10) . . ?
C32 Os3 H2 165(2) . . ?
C31 Os3 H2 72(2) . . ?
C33 Os3 H2 90.7(19) . . ?
C3 Os3 H2 89(2) . . ?
C2 Os3 H2 107(2) . . ?
Os1 Os3 H2 85.0(19) . . ?
Os2 Os3 H2 42(2) . . ?
C2 O1 C5 105.1(7) . . ?
O1 C2 C3 110.9(7) . . ?
O1 C2 Os1 132.9(6) . . ?
C3 C2 Os1 116.2(6) . . ?
O1 C2 Os3 121.5(6) . . ?
C3 C2 Os3 69.7(5) . . ?
Os1 C2 Os3 76.4(3) . . ?
C2 C3 C4 106.4(7) . . ?
C2 C3 Os2 110.9(5) . . ?
C4 C3 Os2 141.0(6) . . ?
C2 C3 Os3 76.1(5) . . ?
C4 C3 Os3 120.4(6) . . ?
Os2 C3 Os3 80.1(3) . . ?
C5 C4 C3 104.4(8) . . ?
C5 C4 H4 127.8 . . ?
C3 C4 H4 127.8 . . ?
C4 C5 O1 113.2(8) . . ?
C4 C5 H5 123.4 . . ?
O1 C5 H5 123.4 . . ?
O11 C11 Os1 176.5(10) . . ?
O12 C12 Os1 174.0(10) . . ?
O13 C13 Os1 178.1(9) . . ?
O21 C21 Os2 177.9(9) . . ?
O22 C22 Os2 178.8(9) . . ?
O23 C23 Os2 176.8(10) . . ?
O31 C31 Os3 176.7(9) . . ?
O32 C32 Os3 179.3(8) . . ?
O33 C33 Os3 179.4(11) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         1.855
_refine_diff_density_min         -3.305
_refine_diff_density_rms         0.383
