# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

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

data_ahg17_J35_0msp1_a
_database_code_depnum_ccdc_archive 'CCDC 1968966'
_audit_update_record             
;
2019-11-28 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H32 F3 N3 O4 Os S'
_chemical_formula_weight         777.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.4840(6)
_cell_length_b                   14.3590(8)
_cell_length_c                   17.8290(10)
_cell_angle_alpha                90
_cell_angle_beta                 96.510(2)
_cell_angle_gamma                90
_cell_volume                     2921.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9696
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      30.55

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_F_000             1536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.497
_shelx_estimated_absorpt_T_min   0.388
_shelx_estimated_absorpt_T_max   0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4737
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'high brilliance microfocus sealed tube '
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω-scans and phi scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            113650
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.826
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_full        26.500
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6447
_reflns_number_gt                5973
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 2017.3 (Bruker AXS Inc.)'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc.)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2-version 1.2.10'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0098P)²+6.0630P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6447
_refine_ls_number_parameters     384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0394
_refine_ls_wR_factor_gt          0.0384
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.52943(2) 0.76757(2) 0.25548(2) 0.01117(3) Uani 1 1 d . . . . .
N1 N 0.45112(17) 0.82011(13) 0.15262(11) 0.0137(4) Uani 1 1 d . . . . .
C1 C 0.5499(2) 0.88930(17) 0.33186(13) 0.0154(5) Uani 1 1 d . . . . .
C2 C 0.5462(2) 0.80594(18) 0.37427(13) 0.0154(5) Uani 1 1 d . . . . .
H2 H 0.477765 0.795348 0.403250 0.018 Uiso 1 1 calc R U . . .
C3 C 0.6238(2) 0.73048(19) 0.36601(13) 0.0171(5) Uani 1 1 d . . . . .
H3 H 0.608900 0.668818 0.389190 0.021 Uiso 1 1 calc R U . . .
C4 C 0.7074(2) 0.73724(18) 0.31305(14) 0.0170(5) Uani 1 1 d . . . . .
C5 C 0.7164(2) 0.82068(18) 0.27183(14) 0.0169(5) Uani 1 1 d . . . . .
H5 H 0.763485 0.821227 0.227966 0.020 Uiso 1 1 calc R U . . .
C6 C 0.6348(2) 0.89315(17) 0.27937(13) 0.0153(5) Uani 1 1 d . . . . .
H6 H 0.628167 0.944157 0.240936 0.018 Uiso 1 1 calc R U . . .
C7 C 0.4709(2) 0.97200(18) 0.34058(15) 0.0202(5) Uani 1 1 d . . . . .
H7 H 0.457602 1.004172 0.290598 0.024 Uiso 1 1 calc R U . . .
C8 C 0.3511(2) 0.9467(2) 0.3642(2) 0.0350(7) Uani 1 1 d . . . . .
H8A H 0.302840 1.002891 0.364473 0.053 Uiso 1 1 calc R U . . .
H8B H 0.361226 0.919248 0.414812 0.053 Uiso 1 1 calc R U . . .
H8C H 0.312498 0.901572 0.328297 0.053 Uiso 1 1 calc R U . . .
C9 C 0.5351(2) 1.0401(2) 0.39697(16) 0.0258(6) Uani 1 1 d . . . . .
H9A H 0.607766 1.060760 0.378110 0.039 Uiso 1 1 calc R U . . .
H9B H 0.553822 1.009045 0.445797 0.039 Uiso 1 1 calc R U . . .
H9C H 0.484925 1.094128 0.403117 0.039 Uiso 1 1 calc R U . . .
C10 C 0.7829(2) 0.65484(19) 0.29867(15) 0.0227(6) Uani 1 1 d . . . . .
H10A H 0.811396 0.661567 0.249182 0.034 Uiso 1 1 calc R U . . .
H10B H 0.736653 0.597560 0.299506 0.034 Uiso 1 1 calc R U . . .
H10C H 0.849765 0.651758 0.337958 0.034 Uiso 1 1 calc R U . . .
C11 C 0.35593(19) 0.73395(17) 0.25794(13) 0.0136(4) Uani 1 1 d . . . . .
C12 C 0.3073(2) 0.68235(17) 0.31332(13) 0.0153(5) Uani 1 1 d . . . . .
H12 H 0.356809 0.661185 0.356254 0.018 Uiso 1 1 calc R U . . .
C13 C 0.1881(2) 0.66127(18) 0.30697(14) 0.0165(5) Uani 1 1 d . . . . .
C14 C 0.1132(2) 0.69448(18) 0.24608(14) 0.0184(5) Uani 1 1 d . . . . .
H14 H 0.031609 0.681819 0.242881 0.022 Uiso 1 1 calc R U . . .
C15 C 0.1573(2) 0.74565(18) 0.19048(14) 0.0184(5) Uani 1 1 d . . . . .
H15 H 0.106390 0.768642 0.148873 0.022 Uiso 1 1 calc R U . . .
C16 C 0.2778(2) 0.76356(17) 0.19577(13) 0.0147(5) Uani 1 1 d . . . . .
C17 C 0.3329(2) 0.81202(16) 0.13714(13) 0.0138(5) Uani 1 1 d . . . . .
C18 C 0.2754(2) 0.84520(18) 0.06886(14) 0.0184(5) Uani 1 1 d . . . . .
H18 H 0.192577 0.840933 0.058684 0.022 Uiso 1 1 calc R U . . .
C19 C 0.3409(2) 0.88423(18) 0.01652(14) 0.0212(5) Uani 1 1 d . . . . .
H19 H 0.303185 0.907562 -0.029846 0.025 Uiso 1 1 calc R U . . .
C20 C 0.4611(2) 0.88923(17) 0.03169(14) 0.0192(5) Uani 1 1 d . . . . .
H20 H 0.507118 0.914192 -0.004537 0.023 Uiso 1 1 calc R U . . .
C21 C 0.5134(2) 0.85744(17) 0.10027(14) 0.0163(5) Uani 1 1 d . . . . .
H21 H 0.596100 0.861952 0.111084 0.020 Uiso 1 1 calc R U . . .
O1 O 0.04280(16) 0.57461(14) 0.36199(11) 0.0265(4) Uani 1 1 d . . . . .
C22 C 0.1438(2) 0.60061(18) 0.36394(14) 0.0195(5) Uani 1 1 d . . . . .
H22 H 0.197807 0.580407 0.405023 0.023 Uiso 1 1 calc R U . . .
N23 N 0.54135(17) 0.64288(14) 0.19256(11) 0.0138(4) Uani 1 1 d . . . . .
C24 C 0.4874(2) 0.56279(17) 0.20827(14) 0.0175(5) Uani 1 1 d . . . . .
H24 H 0.440210 0.563181 0.248719 0.021 Uiso 1 1 calc R U . . .
C25 C 0.4962(2) 0.48144(18) 0.16993(15) 0.0202(5) Uani 1 1 d . . . . .
H25 H 0.455906 0.427585 0.184143 0.024 Uiso 1 1 calc R U . . .
C26 C 0.5651(2) 0.47687(18) 0.10897(14) 0.0180(5) Uani 1 1 d . . . . .
C27 C 0.6244(2) 0.55949(18) 0.09432(14) 0.0174(5) Uani 1 1 d . . . . .
H27 H 0.674719 0.560651 0.055529 0.021 Uiso 1 1 calc R U . . .
C28 C 0.6101(2) 0.63821(18) 0.13567(14) 0.0167(5) Uani 1 1 d . . . . .
H28 H 0.650892 0.692875 0.123783 0.020 Uiso 1 1 calc R U . . .
N29 N 0.5717(2) 0.39855(16) 0.06798(13) 0.0254(5) Uani 1 1 d . . . . .
C30 C 0.5019(3) 0.3175(2) 0.08248(19) 0.0363(7) Uani 1 1 d . . . . .
H30A H 0.511192 0.269572 0.044473 0.054 Uiso 1 1 calc R U . . .
H30B H 0.419175 0.335384 0.079940 0.054 Uiso 1 1 calc R U . . .
H30C H 0.528156 0.292828 0.132822 0.054 Uiso 1 1 calc R U . . .
C31 C 0.6540(3) 0.3912(2) 0.01190(16) 0.0290(6) Uani 1 1 d . . . . .
H31A H 0.647737 0.329217 -0.011245 0.044 Uiso 1 1 calc R U . . .
H31B H 0.733915 0.400701 0.036289 0.044 Uiso 1 1 calc R U . . .
H31C H 0.635602 0.438678 -0.027130 0.044 Uiso 1 1 calc R U . . .
C99 C 0.3874(3) 0.5719(2) 0.58177(17) 0.0291(6) Uani 1 1 d . . . . .
F1 F 0.30423(19) 0.54078(13) 0.62270(13) 0.0514(6) Uani 1 1 d . . . . .
F2 F 0.49071(18) 0.55553(13) 0.62137(11) 0.0444(5) Uani 1 1 d . . . . .
F3 F 0.38153(17) 0.52021(13) 0.51943(12) 0.0452(5) Uani 1 1 d . . . . .
S1 S 0.36693(5) 0.69494(5) 0.56042(3) 0.01911(12) Uani 1 1 d . . . . .
O2 O 0.37124(17) 0.73633(14) 0.63403(10) 0.0253(4) Uani 1 1 d . . . . .
O3 O 0.25339(18) 0.69800(18) 0.51723(13) 0.0404(5) Uani 1 1 d . . . . .
O4 O 0.46527(17) 0.71540(15) 0.51990(11) 0.0288(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C11 2.055(2) . ?
Os1 N1 2.0896(19) . ?
Os1 N23 2.125(2) . ?
Os1 C2 2.176(2) . ?
Os1 C6 2.186(2) . ?
Os1 C3 2.204(2) . ?
Os1 C1 2.212(2) . ?
Os1 C4 2.224(2) . ?
Os1 C5 2.266(2) . ?
N1 C21 1.349(3) . ?
N1 C17 1.359(3) . ?
C1 C2 1.419(3) . ?
C1 C6 1.427(3) . ?
C1 C7 1.513(3) . ?
C2 C3 1.421(4) . ?
C2 H2 1.0000 . ?
C3 C4 1.424(3) . ?
C3 H3 1.0000 . ?
C4 C5 1.416(4) . ?
C4 C10 1.506(4) . ?
C5 C6 1.417(3) . ?
C5 H5 1.0000 . ?
C6 H6 1.0000 . ?
C7 C8 1.527(4) . ?
C7 C9 1.531(4) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.400(3) . ?
C11 C16 1.410(3) . ?
C12 C13 1.395(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(3) . ?
C13 C22 1.472(3) . ?
C14 C15 1.376(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.401(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.458(3) . ?
C17 C18 1.401(3) . ?
C18 C19 1.382(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.377(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.377(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
O1 C22 1.215(3) . ?
C22 H22 0.9500 . ?
N23 C24 1.351(3) . ?
N23 C28 1.356(3) . ?
C24 C25 1.363(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.417(4) . ?
C25 H25 0.9500 . ?
C26 N29 1.348(3) . ?
C26 C27 1.407(4) . ?
C27 C28 1.370(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
N29 C30 1.454(4) . ?
N29 C31 1.455(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C99 F2 1.331(4) . ?
C99 F3 1.332(3) . ?
C99 F1 1.343(3) . ?
C99 S1 1.817(3) . ?
S1 O2 1.4363(19) . ?
S1 O3 1.438(2) . ?
S1 O4 1.4383(19) . ?

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 N1 77.39(9) . . ?
C11 Os1 N23 86.21(8) . . ?
N1 Os1 N23 83.57(8) . . ?
C11 Os1 C2 91.02(9) . . ?
N1 Os1 C2 138.13(9) . . ?
N23 Os1 C2 136.31(9) . . ?
C11 Os1 C6 134.92(9) . . ?
N1 Os1 C6 92.69(8) . . ?
N23 Os1 C6 136.90(8) . . ?
C2 Os1 C6 67.39(9) . . ?
C11 Os1 C3 107.67(9) . . ?
N1 Os1 C3 172.30(9) . . ?
N23 Os1 C3 102.35(9) . . ?
C2 Os1 C3 37.85(9) . . ?
C6 Os1 C3 79.63(9) . . ?
C11 Os1 C1 102.02(9) . . ?
N1 Os1 C1 105.08(8) . . ?
N23 Os1 C1 169.08(8) . . ?
C2 Os1 C1 37.73(9) . . ?
C6 Os1 C1 37.86(9) . . ?
C3 Os1 C1 68.48(9) . . ?
C11 Os1 C4 141.87(9) . . ?
N1 Os1 C4 139.24(8) . . ?
N23 Os1 C4 88.16(8) . . ?
C2 Os1 C4 67.97(9) . . ?
C6 Os1 C4 67.18(9) . . ?
C3 Os1 C4 37.53(9) . . ?
C1 Os1 C4 80.94(9) . . ?
C11 Os1 C5 169.41(9) . . ?
N1 Os1 C5 107.38(8) . . ?
N23 Os1 C5 103.57(8) . . ?
C2 Os1 C5 79.13(9) . . ?
C6 Os1 C5 37.05(9) . . ?
C3 Os1 C5 66.65(9) . . ?
C1 Os1 C5 67.77(9) . . ?
C4 Os1 C5 36.74(9) . . ?
C21 N1 C17 119.3(2) . . ?
C21 N1 Os1 122.78(16) . . ?
C17 N1 Os1 117.90(15) . . ?
C2 C1 C6 116.5(2) . . ?
C2 C1 C7 123.6(2) . . ?
C6 C1 C7 119.9(2) . . ?
C2 C1 Os1 69.76(14) . . ?
C6 C1 Os1 70.10(13) . . ?
C7 C1 Os1 131.32(17) . . ?
C1 C2 C3 122.1(2) . . ?
C1 C2 Os1 72.52(13) . . ?
C3 C2 Os1 72.14(13) . . ?
C1 C2 H2 118.4 . . ?
C3 C2 H2 118.4 . . ?
Os1 C2 H2 118.4 . . ?
C2 C3 C4 119.6(2) . . ?
C2 C3 Os1 70.00(13) . . ?
C4 C3 Os1 71.99(14) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
Os1 C3 H3 119.6 . . ?
C5 C4 C3 119.8(2) . . ?
C5 C4 C10 120.0(2) . . ?
C3 C4 C10 120.3(2) . . ?
C5 C4 Os1 73.26(14) . . ?
C3 C4 Os1 70.48(13) . . ?
C10 C4 Os1 126.30(17) . . ?
C4 C5 C6 119.0(2) . . ?
C4 C5 Os1 70.00(13) . . ?
C6 C5 Os1 68.42(13) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
Os1 C5 H5 119.4 . . ?
C5 C6 C1 122.8(2) . . ?
C5 C6 Os1 74.53(14) . . ?
C1 C6 Os1 72.04(13) . . ?
C5 C6 H6 118.2 . . ?
C1 C6 H6 118.2 . . ?
Os1 C6 H6 118.2 . . ?
C1 C7 C8 114.2(2) . . ?
C1 C7 C9 108.6(2) . . ?
C8 C7 C9 110.7(2) . . ?
C1 C7 H7 107.7 . . ?
C8 C7 H7 107.7 . . ?
C9 C7 H7 107.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 116.4(2) . . ?
C12 C11 Os1 127.17(17) . . ?
C16 C11 Os1 116.37(17) . . ?
C13 C12 C11 121.6(2) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C14 C13 C12 120.2(2) . . ?
C14 C13 C22 120.7(2) . . ?
C12 C13 C22 119.1(2) . . ?
C15 C14 C13 120.0(2) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 119.4(2) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C15 C16 C11 122.2(2) . . ?
C15 C16 C17 123.0(2) . . ?
C11 C16 C17 114.7(2) . . ?
N1 C17 C18 120.6(2) . . ?
N1 C17 C16 113.6(2) . . ?
C18 C17 C16 125.8(2) . . ?
C19 C18 C17 119.0(2) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C20 C19 C18 119.9(2) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 118.9(2) . . ?
C19 C20 H20 120.6 . . ?
C21 C20 H20 120.6 . . ?
N1 C21 C20 122.3(2) . . ?
N1 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
O1 C22 C13 124.4(2) . . ?
O1 C22 H22 117.8 . . ?
C13 C22 H22 117.8 . . ?
C24 N23 C28 115.6(2) . . ?
C24 N23 Os1 123.33(16) . . ?
C28 N23 Os1 120.94(16) . . ?
N23 C24 C25 124.3(2) . . ?
N23 C24 H24 117.8 . . ?
C25 C24 H24 117.8 . . ?
C24 C25 C26 120.3(2) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
N29 C26 C27 123.0(2) . . ?
N29 C26 C25 121.7(2) . . ?
C27 C26 C25 115.3(2) . . ?
C28 C27 C26 120.4(2) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
N23 C28 C27 124.0(2) . . ?
N23 C28 H28 118.0 . . ?
C27 C28 H28 118.0 . . ?
C26 N29 C30 120.3(2) . . ?
C26 N29 C31 121.0(2) . . ?
C30 N29 C31 118.6(2) . . ?
N29 C30 H30A 109.5 . . ?
N29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N29 C31 H31A 109.5 . . ?
N29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
F2 C99 F3 107.6(2) . . ?
F2 C99 F1 107.4(3) . . ?
F3 C99 F1 107.2(2) . . ?
F2 C99 S1 111.7(2) . . ?
F3 C99 S1 112.0(2) . . ?
F1 C99 S1 110.8(2) . . ?
O2 S1 O3 114.33(13) . . ?
O2 S1 O4 115.26(12) . . ?
O3 S1 O4 116.15(13) . . ?
O2 S1 C99 102.75(13) . . ?
O3 S1 C99 103.29(15) . . ?
O4 S1 C99 102.33(13) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C20 H20 O1 0.95 2.47 3.309(3) 147.9 4_675 yes

_refine_diff_density_max         2.011
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.082



####################################################################### 
# 
# 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_ahg9_0msp_a
_database_code_depnum_ccdc_archive 'CCDC 1968967'
_audit_update_record             
;
2019-11-28 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H27 F3 N2 O4 Os S'
_chemical_formula_weight         734.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   12.1045(5)
_cell_length_b                   16.9592(7)
_cell_length_c                   12.9824(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.737(2)
_cell_angle_gamma                90
_cell_volume                     2662.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      30.5

_exptl_crystal_description       lath
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_F_000             1440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    4.928
_shelx_estimated_absorpt_T_min   0.320
_shelx_estimated_absorpt_T_max   0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4489
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'high brilliance microfocus sealed tube '
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω-scans and phi scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            29336
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.977
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8132
_reflns_number_gt                6920
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 2017.3 (Bruker AXS Inc.)'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc.)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 

The triflate anion is disordered over two positions, ca. 50:50%.


;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0182P)²+1.4194P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8132
_refine_ls_number_parameters     428
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0533
_refine_ls_wR_factor_gt          0.0509
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.69402(2) 0.34950(2) 0.31967(2) 0.01435(3) Uani 1 1 d . . . . .
N1 N 0.71091(17) 0.39126(12) 0.47128(16) 0.0177(4) Uani 1 1 d . . . . .
N31 N 0.54034(16) 0.30348(11) 0.36271(15) 0.0146(4) Uani 1 1 d . . . . .
C1 C 0.8729(2) 0.35219(15) 0.2992(2) 0.0269(6) Uani 1 1 d . . . . .
C2 C 0.8463(2) 0.27310(17) 0.3295(3) 0.0377(8) Uani 1 1 d . . . . .
H2 H 0.874191 0.254115 0.398848 0.045 Uiso 1 1 calc R U . . .
C3 C 0.7631(3) 0.23000(18) 0.2769(3) 0.0444(10) Uani 1 1 d . . . . .
H3 H 0.733620 0.181884 0.310651 0.053 Uiso 1 1 calc R U . . .
C4 C 0.7010(3) 0.26337(19) 0.1919(3) 0.0404(9) Uani 1 1 d . . . . .
C5 C 0.7301(3) 0.33894(19) 0.1572(2) 0.0355(7) Uani 1 1 d . . . . .
H5 H 0.680964 0.366005 0.104056 0.043 Uiso 1 1 calc R U . . .
C6 C 0.8161(2) 0.38315(17) 0.2111(2) 0.0273(6) Uani 1 1 d . . . . .
H6 H 0.825277 0.440246 0.194288 0.033 Uiso 1 1 calc R U . . .
C7 C 0.9590(2) 0.39763(17) 0.3632(2) 0.0303(6) Uani 1 1 d . . . . .
H7 H 0.945814 0.386823 0.437324 0.036 Uiso 1 1 calc R U . . .
C8 C 1.0732(3) 0.3666(2) 0.3424(3) 0.0460(9) Uani 1 1 d . . . . .
H8A H 1.089046 0.376412 0.270166 0.069 Uiso 1 1 calc R U . . .
H8B H 1.075999 0.309765 0.356003 0.069 Uiso 1 1 calc R U . . .
H8C H 1.128417 0.393494 0.387474 0.069 Uiso 1 1 calc R U . . .
C9 C 0.9510(3) 0.48644(18) 0.3476(3) 0.0358(7) Uani 1 1 d . . . . .
H9A H 0.966485 0.499372 0.276167 0.054 Uiso 1 1 calc R U . . .
H9B H 1.004945 0.512863 0.394506 0.054 Uiso 1 1 calc R U . . .
H9C H 0.876279 0.504251 0.362134 0.054 Uiso 1 1 calc R U . . .
C10 C 0.6076(3) 0.2174(2) 0.1390(3) 0.0652(14) Uani 1 1 d . . . . .
H10A H 0.558801 0.253716 0.099611 0.098 Uiso 1 1 calc R U . . .
H10B H 0.565450 0.190248 0.190918 0.098 Uiso 1 1 calc R U . . .
H10C H 0.638040 0.178596 0.092203 0.098 Uiso 1 1 calc R U . . .
C11 C 0.61900(19) 0.45846(14) 0.30926(19) 0.0159(5) Uani 1 1 d . . . . .
C12 C 0.5663(2) 0.49305(16) 0.2217(2) 0.0247(6) Uani 1 1 d . . . . .
H12 H 0.560911 0.464151 0.158953 0.030 Uiso 1 1 calc R U . . .
C13 C 0.5219(2) 0.56863(17) 0.2247(3) 0.0327(7) Uani 1 1 d . . . . .
C14 C 0.5299(2) 0.61280(16) 0.3146(3) 0.0375(8) Uani 1 1 d . . . . .
H14 H 0.500913 0.664827 0.315686 0.045 Uiso 1 1 calc R U . . .
C15 C 0.5799(2) 0.58090(16) 0.4018(3) 0.0297(7) Uani 1 1 d . . . . .
H15 H 0.585289 0.610851 0.463643 0.036 Uiso 1 1 calc R U . . .
C16 C 0.6233(2) 0.50436(14) 0.4002(2) 0.0182(5) Uani 1 1 d . . . . .
C17 C 0.6741(2) 0.46541(15) 0.49046(19) 0.0200(5) Uani 1 1 d . . . . .
C18 C 0.6870(3) 0.4965(2) 0.5894(2) 0.0344(7) Uani 1 1 d . . . . .
H18 H 0.661093 0.548144 0.602908 0.041 Uiso 1 1 calc R U . . .
C19 C 0.7373(3) 0.4529(3) 0.6681(2) 0.0508(11) Uani 1 1 d . . . . .
H19 H 0.747163 0.474317 0.735555 0.061 Uiso 1 1 calc R U . . .
C20 C 0.7724(3) 0.3785(2) 0.6475(3) 0.0484(10) Uani 1 1 d . . . . .
H20 H 0.806225 0.347209 0.700844 0.058 Uiso 1 1 calc R U . . .
C21 C 0.7588(2) 0.34910(17) 0.5497(2) 0.0313(7) Uani 1 1 d . . . . .
H21 H 0.783846 0.297179 0.536405 0.038 Uiso 1 1 calc R U . . .
C22 C 0.4632(3) 0.5988(2) 0.1301(3) 0.0508(11) Uani 1 1 d . . . . .
H22 H 0.462247 0.566178 0.070640 0.061 Uiso 1 1 calc R U . . .
O1 O 0.4166(2) 0.66160(15) 0.1225(3) 0.0712(10) Uani 1 1 d . . . . .
C31 C 0.5345(2) 0.25236(14) 0.44147(19) 0.0196(5) Uani 1 1 d . . . . .
H31 H 0.600459 0.239616 0.480595 0.024 Uiso 1 1 calc R U . . .
C32 C 0.4366(2) 0.21768(15) 0.4677(2) 0.0236(5) Uani 1 1 d . . . . .
H32 H 0.435495 0.182687 0.524798 0.028 Uiso 1 1 calc R U . . .
C33 C 0.3405(2) 0.23417(15) 0.4105(2) 0.0237(6) Uani 1 1 d . . . . .
H33 H 0.272494 0.210272 0.426787 0.028 Uiso 1 1 calc R U . . .
C34 C 0.3452(2) 0.28636(15) 0.3288(2) 0.0204(5) Uani 1 1 d . . . . .
H34 H 0.280488 0.298751 0.287749 0.024 Uiso 1 1 calc R U . . .
C35 C 0.4455(2) 0.32012(14) 0.30794(19) 0.0166(5) Uani 1 1 d . . . . .
H35 H 0.447944 0.356654 0.252622 0.020 Uiso 1 1 calc R U . . .
C99 C 0.8519(7) 0.5431(5) 0.9760(8) 0.0266(19) Uani 0.493(7) 1 d D . P A 1
F1 F 0.8418(7) 0.4661(3) 0.9743(6) 0.072(2) Uani 0.493(7) 1 d D . P A 1
F2 F 0.9298(3) 0.5646(4) 0.9138(3) 0.0548(18) Uani 0.493(7) 1 d D . P A 1
F3 F 0.8850(10) 0.5637(6) 1.0727(6) 0.041(2) Uani 0.493(7) 1 d D . P A 1
S1 S 0.7214(5) 0.5908(4) 0.9408(4) 0.0307(11) Uani 0.493(7) 1 d D . P A 1
O2 O 0.7482(7) 0.6724(4) 0.9440(9) 0.094(4) Uani 0.493(7) 1 d D . P A 1
O3 O 0.6524(5) 0.5634(7) 1.0197(5) 0.107(4) Uani 0.493(7) 1 d D . P A 1
O4 O 0.6935(5) 0.5618(5) 0.8394(5) 0.0318(14) Uani 0.493(7) 1 d D . P A 1
C99B C 0.8245(7) 0.5298(5) 0.9754(7) 0.033(3) Uani 0.507(7) 1 d D . P A 2
F1B F 0.7680(6) 0.4695(3) 1.0105(4) 0.0605(18) Uani 0.507(7) 1 d D . P A 2
F2B F 0.8804(5) 0.5030(4) 0.8984(4) 0.073(2) Uani 0.507(7) 1 d D . P A 2
F3B F 0.8994(10) 0.5504(7) 1.0498(8) 0.060(3) Uani 0.507(7) 1 d D . P A 2
S1B S 0.7325(5) 0.6091(3) 0.9371(4) 0.0242(8) Uani 0.507(7) 1 d D . P A 2
O2B O 0.8044(5) 0.6642(3) 0.8903(4) 0.0378(14) Uani 0.507(7) 1 d D . P A 2
O3B O 0.6911(6) 0.6357(4) 1.0309(4) 0.0574(19) Uani 0.507(7) 1 d D . P A 2
O4B O 0.6550(5) 0.5712(4) 0.8678(5) 0.0373(15) Uani 0.507(7) 1 d D . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C11 2.060(2) . ?
Os1 N1 2.093(2) . ?
Os1 N31 2.1169(19) . ?
Os1 C6 2.166(2) . ?
Os1 C5 2.182(3) . ?
Os1 C1 2.194(3) . ?
Os1 C4 2.215(3) . ?
Os1 C2 2.252(3) . ?
Os1 C3 2.271(3) . ?
N1 C21 1.352(3) . ?
N1 C17 1.361(3) . ?
N31 C31 1.345(3) . ?
N31 C35 1.351(3) . ?
C1 C6 1.408(4) . ?
C1 C2 1.438(4) . ?
C1 C7 1.513(4) . ?
C2 C3 1.396(5) . ?
C2 H2 1.0000 . ?
C3 C4 1.423(5) . ?
C3 H3 1.0000 . ?
C4 C5 1.409(5) . ?
C4 C10 1.511(5) . ?
C5 C6 1.438(4) . ?
C5 H5 1.0000 . ?
C6 H6 1.0000 . ?
C7 C8 1.515(4) . ?
C7 C9 1.522(4) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.405(3) . ?
C11 C16 1.413(3) . ?
C12 C13 1.391(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(5) . ?
C13 C22 1.479(4) . ?
C14 C15 1.369(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.401(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.455(4) . ?
C17 C18 1.391(4) . ?
C18 C19 1.379(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.361(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.366(5) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 O1 1.207(4) . ?
C22 H22 0.9500 . ?
C31 C32 1.380(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.379(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.385(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.381(3) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C99 F1 1.313(9) . ?
C99 F2 1.322(9) . ?
C99 F3 1.345(10) . ?
C99 S1 1.814(9) . ?
S1 O2 1.423(7) . ?
S1 O3 1.430(7) . ?
S1 O4 1.431(7) . ?
C99B F2B 1.315(9) . ?
C99B F1B 1.325(9) . ?
C99B F3B 1.337(9) . ?
C99B S1B 1.800(9) . ?
S1B O3B 1.412(7) . ?
S1B O4B 1.422(7) . ?
S1B O2B 1.432(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 Os1 N1 77.36(9) . . ?
C11 Os1 N31 87.58(8) . . ?
N1 Os1 N31 85.65(7) . . ?
C11 Os1 C6 91.90(10) . . ?
N1 Os1 C6 118.92(9) . . ?
N31 Os1 C6 154.70(10) . . ?
C11 Os1 C5 96.78(11) . . ?
N1 Os1 C5 157.24(10) . . ?
N31 Os1 C5 116.34(10) . . ?
C6 Os1 C5 38.62(11) . . ?
C11 Os1 C1 114.06(9) . . ?
N1 Os1 C1 93.10(10) . . ?
N31 Os1 C1 157.54(9) . . ?
C6 Os1 C1 37.66(11) . . ?
C5 Os1 C1 68.95(12) . . ?
C11 Os1 C4 125.09(13) . . ?
N1 Os1 C4 157.23(12) . . ?
N31 Os1 C4 91.15(9) . . ?
C6 Os1 C4 68.59(11) . . ?
C5 Os1 C4 37.36(12) . . ?
C1 Os1 C4 81.36(11) . . ?
C11 Os1 C2 151.25(10) . . ?
N1 Os1 C2 95.66(11) . . ?
N31 Os1 C2 120.02(9) . . ?
C6 Os1 C2 66.82(12) . . ?
C5 Os1 C2 78.84(13) . . ?
C1 Os1 C2 37.71(10) . . ?
C4 Os1 C2 66.56(14) . . ?
C11 Os1 C3 161.89(13) . . ?
N1 Os1 C3 120.74(13) . . ?
N31 Os1 C3 94.24(9) . . ?
C6 Os1 C3 78.79(11) . . ?
C5 Os1 C3 66.27(14) . . ?
C1 Os1 C3 67.17(10) . . ?
C4 Os1 C3 36.95(14) . . ?
C2 Os1 C3 35.94(12) . . ?
C21 N1 C17 118.9(2) . . ?
C21 N1 Os1 123.28(19) . . ?
C17 N1 Os1 117.81(17) . . ?
C31 N31 C35 117.5(2) . . ?
C31 N31 Os1 121.11(16) . . ?
C35 N31 Os1 121.29(16) . . ?
C6 C1 C2 117.6(3) . . ?
C6 C1 C7 123.6(2) . . ?
C2 C1 C7 118.9(3) . . ?
C6 C1 Os1 70.10(15) . . ?
C2 C1 Os1 73.33(15) . . ?
C7 C1 Os1 127.05(19) . . ?
C3 C2 C1 121.4(3) . . ?
C3 C2 Os1 72.78(17) . . ?
C1 C2 Os1 68.96(15) . . ?
C3 C2 H2 118.4 . . ?
C1 C2 H2 118.4 . . ?
Os1 C2 H2 118.4 . . ?
C2 C3 C4 120.9(3) . . ?
C2 C3 Os1 71.28(16) . . ?
C4 C3 Os1 69.37(16) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
Os1 C3 H3 118.5 . . ?
C5 C4 C3 118.7(3) . . ?
C5 C4 C10 121.1(4) . . ?
C3 C4 C10 120.2(3) . . ?
C5 C4 Os1 70.05(16) . . ?
C3 C4 Os1 73.68(18) . . ?
C10 C4 Os1 128.7(2) . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 Os1 72.58(17) . . ?
C6 C5 Os1 70.10(15) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
Os1 C5 H5 119.3 . . ?
C1 C6 C5 121.0(3) . . ?
C1 C6 Os1 72.24(15) . . ?
C5 C6 Os1 71.28(15) . . ?
C1 C6 H6 118.9 . . ?
C5 C6 H6 118.9 . . ?
Os1 C6 H6 118.9 . . ?
C1 C7 C8 109.6(3) . . ?
C1 C7 C9 113.1(2) . . ?
C8 C7 C9 111.9(2) . . ?
C1 C7 H7 107.3 . . ?
C8 C7 H7 107.3 . . ?
C9 C7 H7 107.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 116.3(2) . . ?
C12 C11 Os1 127.52(19) . . ?
C16 C11 Os1 116.16(18) . . ?
C13 C12 C11 121.6(3) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C14 C13 C12 120.6(3) . . ?
C14 C13 C22 121.5(3) . . ?
C12 C13 C22 117.8(3) . . ?
C15 C14 C13 119.5(3) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 121.6(3) . . ?
C15 C16 C17 123.6(2) . . ?
C11 C16 C17 114.8(2) . . ?
N1 C17 C18 119.7(3) . . ?
N1 C17 C16 113.7(2) . . ?
C18 C17 C16 126.6(3) . . ?
C19 C18 C17 120.5(3) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
C19 C20 C21 119.8(3) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
N1 C21 C20 122.3(3) . . ?
N1 C21 H21 118.8 . . ?
C20 C21 H21 118.8 . . ?
O1 C22 C13 125.3(4) . . ?
O1 C22 H22 117.4 . . ?
C13 C22 H22 117.4 . . ?
N31 C31 C32 122.6(2) . . ?
N31 C31 H31 118.7 . . ?
C32 C31 H31 118.7 . . ?
C33 C32 C31 119.6(2) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C32 C33 C34 118.5(2) . . ?
C32 C33 H33 120.8 . . ?
C34 C33 H33 120.8 . . ?
C35 C34 C33 119.0(2) . . ?
C35 C34 H34 120.5 . . ?
C33 C34 H34 120.5 . . ?
N31 C35 C34 122.9(2) . . ?
N31 C35 H35 118.6 . . ?
C34 C35 H35 118.6 . . ?
F1 C99 F2 109.4(7) . . ?
F1 C99 F3 107.3(8) . . ?
F2 C99 F3 108.0(8) . . ?
F1 C99 S1 111.1(7) . . ?
F2 C99 S1 111.2(6) . . ?
F3 C99 S1 109.7(8) . . ?
O2 S1 O3 115.8(8) . . ?
O2 S1 O4 113.9(6) . . ?
O3 S1 O4 115.3(6) . . ?
O2 S1 C99 103.4(5) . . ?
O3 S1 C99 101.9(5) . . ?
O4 S1 C99 104.1(5) . . ?
F2B C99B F1B 106.7(8) . . ?
F2B C99B F3B 106.5(8) . . ?
F1B C99B F3B 107.2(8) . . ?
F2B C99B S1B 112.4(6) . . ?
F1B C99B S1B 110.4(6) . . ?
F3B C99B S1B 113.2(8) . . ?
O3B S1B O4B 116.1(6) . . ?
O3B S1B O2B 113.9(5) . . ?
O4B S1B O2B 114.9(5) . . ?
O3B S1B C99B 103.9(5) . . ?
O4B S1B C99B 102.6(5) . . ?
O2B S1B C99B 102.9(5) . . ?

_refine_diff_density_max         0.818
_refine_diff_density_min         -1.738
_refine_diff_density_rms         0.116



####################################################################### 
# 
# 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_AHG_1_0msp_a
_database_code_depnum_ccdc_archive 'CCDC 1968968'
_audit_update_record             
;
2019-11-28 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H22 Cl N O Os'
_chemical_formula_weight         542.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.1387(4)
_cell_length_b                   13.1760(5)
_cell_length_c                   12.5063(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.3700(10)
_cell_angle_gamma                90
_cell_volume                     1834.94(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9376
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      30.58

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_F_000             1048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    7.106
_shelx_estimated_absorpt_T_min   0.203
_shelx_estimated_absorpt_T_max   0.317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4511
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'high brilliance microfocus sealed tube '
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω-scans and phi scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            120198
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.246
_diffrn_reflns_theta_max         30.609
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5630
_reflns_number_gt                5414
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 2017.3 (Bruker AXS Inc.)'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc.)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0114P)²+1.7770P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5630
_refine_ls_number_parameters     238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0146
_refine_ls_R_factor_gt           0.0134
_refine_ls_wR_factor_ref         0.0327
_refine_ls_wR_factor_gt          0.0323
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_restrained_S_all      1.202
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.47077(2) 0.76849(2) 0.26021(2) 0.00707(2) Uani 1 1 d . . . . .
Cl1 Cl 0.57524(4) 0.81963(3) 0.10076(3) 0.01266(7) Uani 1 1 d . . . . .
N1 N 0.63364(12) 0.70011(11) 0.30649(10) 0.0090(2) Uani 1 1 d . . . . .
C1 C 0.41800(15) 0.78593(12) 0.42627(13) 0.0102(3) Uani 1 1 d . . . . .
C2 C 0.32169(15) 0.74320(13) 0.36447(14) 0.0125(3) Uani 1 1 d . . . . .
H2 H 0.294964 0.672241 0.379351 0.015 Uiso 1 1 calc R U . . .
C3 C 0.27773(15) 0.79395(14) 0.27040(14) 0.0145(3) Uani 1 1 d . . . . .
H3 H 0.222155 0.756816 0.220080 0.017 Uiso 1 1 calc R U . . .
C4 C 0.32845(16) 0.88581(14) 0.23726(14) 0.0151(3) Uani 1 1 d . . . . .
C5 C 0.42154(16) 0.93074(13) 0.30236(13) 0.0133(3) Uani 1 1 d . . . . .
H5 H 0.469664 0.987324 0.271701 0.016 Uiso 1 1 calc R U . . .
C6 C 0.46464(15) 0.88304(13) 0.39505(13) 0.0114(3) Uani 1 1 d . . . . .
H6 H 0.541978 0.907072 0.428489 0.014 Uiso 1 1 calc R U . . .
C7 C 0.47155(17) 0.73498(13) 0.52460(14) 0.0142(3) Uani 1 1 d . . . . .
H7 H 0.560251 0.746649 0.524301 0.017 Uiso 1 1 calc R U . . .
C8 C 0.42391(18) 0.78459(15) 0.62583(14) 0.0180(3) Uani 1 1 d . . . . .
H8A H 0.434611 0.858297 0.621588 0.027 Uiso 1 1 calc R U . . .
H8B H 0.468242 0.758351 0.688561 0.027 Uiso 1 1 calc R U . . .
H8C H 0.338369 0.768892 0.632141 0.027 Uiso 1 1 calc R U . . .
C9 C 0.4513(2) 0.62113(15) 0.52690(16) 0.0275(5) Uani 1 1 d . . . . .
H9A H 0.365646 0.607151 0.535393 0.041 Uiso 1 1 calc R U . . .
H9B H 0.497195 0.591500 0.587010 0.041 Uiso 1 1 calc R U . . .
H9C H 0.477999 0.591193 0.459786 0.041 Uiso 1 1 calc R U . . .
C10 C 0.2827(2) 0.93934(17) 0.13847(16) 0.0258(4) Uani 1 1 d . . . . .
H10A H 0.349756 0.972595 0.103176 0.039 Uiso 1 1 calc R U . . .
H10B H 0.223251 0.990426 0.158222 0.039 Uiso 1 1 calc R U . . .
H10C H 0.245227 0.889951 0.089508 0.039 Uiso 1 1 calc R U . . .
C11 C 0.45697(14) 0.62718(12) 0.19159(12) 0.0085(3) Uani 1 1 d . . . . .
C12 C 0.36813(14) 0.59203(12) 0.11981(12) 0.0095(3) Uani 1 1 d . . . . .
H12 H 0.305692 0.636744 0.097012 0.011 Uiso 1 1 calc R U . . .
C13 C 0.36917(14) 0.49246(12) 0.08085(12) 0.0093(3) Uani 1 1 d . . . . .
C14 C 0.45665(14) 0.42340(12) 0.11605(13) 0.0104(3) Uani 1 1 d . . . . .
H14 H 0.453937 0.354811 0.092706 0.013 Uiso 1 1 calc R U . . .
C15 C 0.54724(14) 0.45609(12) 0.18527(13) 0.0105(3) Uani 1 1 d . . . . .
H15 H 0.607682 0.410146 0.209620 0.013 Uiso 1 1 calc R U . . .
C16 C 0.54933(14) 0.55734(12) 0.21927(12) 0.0090(3) Uani 1 1 d . . . . .
C17 C 0.64908(14) 0.60038(12) 0.28208(12) 0.0093(3) Uani 1 1 d . . . . .
C18 C 0.75361(15) 0.54888(13) 0.31398(13) 0.0119(3) Uani 1 1 d . . . . .
H18 H 0.763971 0.479579 0.295389 0.014 Uiso 1 1 calc R U . . .
C19 C 0.84170(15) 0.59911(14) 0.37258(13) 0.0134(3) Uani 1 1 d . . . . .
H19 H 0.912272 0.564423 0.396146 0.016 Uiso 1 1 calc R U . . .
C20 C 0.82578(15) 0.70138(14) 0.39673(13) 0.0132(3) Uani 1 1 d . . . . .
H20 H 0.885383 0.737537 0.436768 0.016 Uiso 1 1 calc R U . . .
C21 C 0.72167(15) 0.74945(13) 0.36141(13) 0.0113(3) Uani 1 1 d . . . . .
H21 H 0.711809 0.819609 0.376337 0.014 Uiso 1 1 calc R U . . .
C22 C 0.28360(14) 0.45843(12) -0.00309(13) 0.0109(3) Uani 1 1 d . . . . .
H22 H 0.287295 0.389430 -0.024818 0.013 Uiso 1 1 calc R U . . .
O1 O 0.20831(11) 0.51236(10) -0.04676(10) 0.0160(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C11 2.0543(15) . ?
Os1 N1 2.0946(14) . ?
Os1 C2 2.1615(17) . ?
Os1 C3 2.1830(17) . ?
Os1 C1 2.1839(16) . ?
Os1 C4 2.2279(17) . ?
Os1 C6 2.2655(16) . ?
Os1 C5 2.2722(16) . ?
Os1 Cl1 2.4281(4) . ?
N1 C21 1.350(2) . ?
N1 C17 1.361(2) . ?
C1 C2 1.423(2) . ?
C1 C6 1.438(2) . ?
C1 C7 1.511(2) . ?
C2 C3 1.430(3) . ?
C2 H2 1.0000 . ?
C3 C4 1.403(3) . ?
C3 H3 1.0000 . ?
C4 C5 1.431(3) . ?
C4 C10 1.501(3) . ?
C5 C6 1.394(2) . ?
C5 H5 1.0000 . ?
C6 H6 1.0000 . ?
C7 C9 1.517(3) . ?
C7 C8 1.531(2) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.399(2) . ?
C11 C16 1.417(2) . ?
C12 C13 1.400(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.397(2) . ?
C13 C22 1.471(2) . ?
C14 C15 1.383(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.400(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.460(2) . ?
C17 C18 1.397(2) . ?
C18 C19 1.380(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.393(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.384(2) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 O1 1.218(2) . ?
C22 H22 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 Os1 N1 77.37(6) . . ?
C11 Os1 C2 93.52(6) . . ?
N1 Os1 C2 116.09(6) . . ?
C11 Os1 C3 95.72(6) . . ?
N1 Os1 C3 153.87(6) . . ?
C2 Os1 C3 38.42(7) . . ?
C11 Os1 C1 118.26(6) . . ?
N1 Os1 C1 91.92(6) . . ?
C2 Os1 C1 38.23(6) . . ?
C3 Os1 C1 68.93(6) . . ?
C11 Os1 C4 121.95(7) . . ?
N1 Os1 C4 160.55(6) . . ?
C2 Os1 C4 68.29(7) . . ?
C3 Os1 C4 37.06(7) . . ?
C1 Os1 C4 80.95(6) . . ?
C11 Os1 C6 155.72(6) . . ?
N1 Os1 C6 97.02(6) . . ?
C2 Os1 C6 67.44(6) . . ?
C3 Os1 C6 78.86(6) . . ?
C1 Os1 C6 37.67(6) . . ?
C4 Os1 C6 66.40(6) . . ?
C11 Os1 C5 159.00(6) . . ?
N1 Os1 C5 123.56(6) . . ?
C2 Os1 C5 79.16(6) . . ?
C3 Os1 C5 66.32(7) . . ?
C1 Os1 C5 66.95(6) . . ?
C4 Os1 C5 37.07(6) . . ?
C6 Os1 C5 35.78(6) . . ?
C11 Os1 Cl1 86.61(4) . . ?
N1 Os1 Cl1 85.26(4) . . ?
C2 Os1 Cl1 158.18(5) . . ?
C3 Os1 Cl1 119.82(5) . . ?
C1 Os1 Cl1 153.76(4) . . ?
C4 Os1 Cl1 93.16(5) . . ?
C6 Os1 Cl1 116.74(4) . . ?
C5 Os1 Cl1 93.01(4) . . ?
C21 N1 C17 119.00(14) . . ?
C21 N1 Os1 123.16(11) . . ?
C17 N1 Os1 117.82(11) . . ?
C2 C1 C6 118.49(15) . . ?
C2 C1 C7 122.94(15) . . ?
C6 C1 C7 118.55(15) . . ?
C2 C1 Os1 70.03(9) . . ?
C6 C1 Os1 74.24(9) . . ?
C7 C1 Os1 128.10(11) . . ?
C1 C2 C3 120.05(15) . . ?
C1 C2 Os1 71.74(9) . . ?
C3 C2 Os1 71.61(10) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
Os1 C2 H2 119.5 . . ?
C4 C3 C2 120.96(16) . . ?
C4 C3 Os1 73.21(10) . . ?
C2 C3 Os1 69.98(9) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
Os1 C3 H3 118.9 . . ?
C3 C4 C5 118.71(16) . . ?
C3 C4 C10 121.16(18) . . ?
C5 C4 C10 120.06(17) . . ?
C3 C4 Os1 69.73(10) . . ?
C5 C4 Os1 73.15(10) . . ?
C10 C4 Os1 131.19(13) . . ?
C6 C5 C4 121.14(16) . . ?
C6 C5 Os1 71.85(9) . . ?
C4 C5 Os1 69.78(9) . . ?
C6 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
Os1 C5 H5 118.6 . . ?
C5 C6 C1 120.49(15) . . ?
C5 C6 Os1 72.38(9) . . ?
C1 C6 Os1 68.09(9) . . ?
C5 C6 H6 118.8 . . ?
C1 C6 H6 118.8 . . ?
Os1 C6 H6 118.8 . . ?
C1 C7 C9 113.50(16) . . ?
C1 C7 C8 110.20(14) . . ?
C9 C7 C8 110.60(15) . . ?
C1 C7 H7 107.4 . . ?
C9 C7 H7 107.4 . . ?
C8 C7 H7 107.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 116.11(14) . . ?
C12 C11 Os1 127.79(12) . . ?
C16 C11 Os1 116.09(11) . . ?
C11 C12 C13 121.47(15) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C14 C13 C12 120.83(15) . . ?
C14 C13 C22 117.50(14) . . ?
C12 C13 C22 121.57(15) . . ?
C15 C14 C13 119.19(15) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C16 119.57(15) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C11 122.54(15) . . ?
C15 C16 C17 122.71(14) . . ?
C11 C16 C17 114.71(14) . . ?
N1 C17 C18 120.91(15) . . ?
N1 C17 C16 113.39(14) . . ?
C18 C17 C16 125.67(15) . . ?
C19 C18 C17 119.73(16) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 119.11(16) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
C21 C20 C19 118.90(16) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
N1 C21 C20 122.32(16) . . ?
N1 C21 H21 118.8 . . ?
C20 C21 H21 118.8 . . ?
O1 C22 C13 124.71(15) . . ?
O1 C22 H22 117.6 . . ?
C13 C22 H22 117.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C21 H21 O1 0.95 2.41 3.346(2) 166.8 4_676 yes

_refine_diff_density_max         0.505
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.113



