# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_al_003_c2_auto
_database_code_depnum_ccdc_archive 'CCDC 2351192'
loop_
_audit_author_name
_audit_author_address
'Sheridon Kelly'
;University of California, Berkeley
United States of America
;
_audit_update_record             
;
2024-06-03 deposited with the CCDC.	2024-06-26 downloaded from the CCDC.
;
_audit_creation_date             2024-06-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H51 Os Ta'
_chemical_formula_sum            'C25 H51 Os Ta'
_chemical_formula_weight         722.80
_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'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.7258(4)
_cell_length_b                   16.5130(2)
_cell_length_c                   19.8168(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.405(2)
_cell_angle_gamma                90
_cell_volume                     5618.14(19)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    32863
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.0350
_cell_measurement_theta_min      2.6670
_shelx_estimated_absorpt_T_max   0.921
_shelx_estimated_absorpt_T_min   0.850
_exptl_absorpt_coefficient_mu    8.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         1.851
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      8.00  98.00   0.50   14.35    --   24.81  63.00-111.00  180
  2  ω    -47.00  42.00   0.50   14.35    --   24.81 -63.00 111.00  178
  3  ω    -97.00  -8.00   0.50   14.35    --  -25.20 -63.00 111.00  178
  4  ω     10.00  38.00   0.50   14.35    --   24.81  57.00  30.00   56
  5  ω    -50.00 -13.00   0.50   14.35    --   24.81 -19.00   0.00   74
  6  ω     10.00  38.00   0.50   14.35    --   24.81  57.00 120.00   56
  7  ω    -50.00 -13.00   0.50   14.35    --   24.81 -19.00 -30.00   74
  8  ω    -50.00 -13.00   0.50   14.35    --   24.81 -19.00-180.00   74
  9  ω      9.00  35.00   0.50   14.35    --   24.81  59.00  74.00   52
 10  ω    -77.00 -39.00   0.50   14.35    --  -25.20 134.00 -89.15   76
 11  ω    -50.00 -13.00   0.50   14.35    --   24.81 -19.00 150.00   74
 12  ω    -16.00  48.00   0.50   14.35    --   24.81 -77.00-120.00  128
 13  ω    -82.00 -51.00   0.50   14.35    --  -25.20 141.00 -51.73   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0179348000
_diffrn_orient_matrix_UB_12      0.0315698000
_diffrn_orient_matrix_UB_13      -0.0226626000
_diffrn_orient_matrix_UB_21      -0.0317779000
_diffrn_orient_matrix_UB_22      0.0000564000
_diffrn_orient_matrix_UB_23      0.0158099000
_diffrn_orient_matrix_UB_31      0.0194381000
_diffrn_orient_matrix_UB_32      0.0291372000
_diffrn_orient_matrix_UB_33      0.0244815000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4817
_reflns_number_total             5159
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5159
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0165
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0099P)²+15.0761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0337
_refine_ls_wR_factor_ref         0.0342
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C16(H16A,H16B), C11(H11A,H11B)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C14(H14A,H14B,
 H14C), C6(H6A,H6B,H6C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C7(H7A,H7B,
 H7C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C24(H24A,H24B,
 H24C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.20168(2) 0.47664(2) 0.38343(2) 0.01349(4) Uani 1 1 d . . . . .
Ta1 Ta 0.34265(2) 0.48736(2) 0.44099(2) 0.01391(4) Uani 1 1 d . . . . .
C17 C 0.36084(18) 0.68535(16) 0.40264(15) 0.0232(6) Uani 1 1 d . . . . .
C1 C 0.09806(16) 0.39847(16) 0.34046(15) 0.0193(6) Uani 1 1 d . . . . .
C21 C 0.41588(16) 0.41921(16) 0.39149(15) 0.0186(6) Uani 1 1 d . . . . .
H21A H 0.425032 0.455401 0.355800 0.022 Uiso 1 1 calc R U . . .
H21B H 0.465099 0.416247 0.426352 0.022 Uiso 1 1 calc R U . . .
C5 C 0.08278(15) 0.44864(16) 0.39537(14) 0.0172(6) Uani 1 1 d . . . . .
C16 C 0.38642(16) 0.60829(16) 0.44558(15) 0.0211(6) Uani 1 1 d . . . . .
H16A H 0.388819 0.625051 0.492978 0.025 Uiso 1 1 calc R U . . .
H16B H 0.440189 0.601235 0.443715 0.025 Uiso 1 1 calc R U . . .
C11 C 0.37405(16) 0.44817(17) 0.54740(14) 0.0214(6) Uani 1 1 d . . . . .
H11A H 0.378968 0.389832 0.544716 0.026 Uiso 1 1 calc R U . . .
H11B H 0.426599 0.468331 0.565507 0.026 Uiso 1 1 calc R U . . .
C22 C 0.40770(17) 0.33524(16) 0.35663(15) 0.0210(6) Uani 1 1 d . . . . .
C4 C 0.08494(16) 0.53140(16) 0.37388(15) 0.0179(6) Uani 1 1 d . . . . .
C3 C 0.10158(16) 0.53265(17) 0.30715(15) 0.0194(6) Uani 1 1 d . . . . .
C23 C 0.48633(18) 0.30920(18) 0.34486(17) 0.0281(7) Uani 1 1 d . . . . .
H23A H 0.504320 0.349503 0.317622 0.042 Uiso 1 1 calc R U . . .
H23B H 0.480493 0.258393 0.320569 0.042 Uiso 1 1 calc R U . . .
H23C H 0.523472 0.303380 0.389008 0.042 Uiso 1 1 calc R U . . .
C10 C 0.06136(17) 0.42006(17) 0.45966(15) 0.0232(6) Uani 1 1 d . . . . .
H10A H 0.084742 0.368170 0.473020 0.035 Uiso 1 1 calc R U . . .
H10B H 0.005754 0.415449 0.450638 0.035 Uiso 1 1 calc R U . . .
H10C H 0.079814 0.458205 0.496647 0.035 Uiso 1 1 calc R U . . .
C2 C 0.10926(16) 0.45004(17) 0.28657(15) 0.0206(6) Uani 1 1 d . . . . .
C9 C 0.06872(18) 0.60342(17) 0.41435(16) 0.0257(7) Uani 1 1 d . . . . .
H9A H 0.090136 0.594235 0.463211 0.039 Uiso 1 1 calc R U . . .
H9B H 0.013470 0.611315 0.405605 0.039 Uiso 1 1 calc R U . . .
H9C H 0.092176 0.650749 0.400125 0.039 Uiso 1 1 calc R U . . .
C14 C 0.3927(2) 0.4476(2) 0.67737(16) 0.0372(8) Uani 1 1 d . . . . .
H14A H 0.412050 0.393145 0.679299 0.056 Uiso 1 1 calc R U . . .
H14B H 0.367592 0.455973 0.714502 0.056 Uiso 1 1 calc R U . . .
H14C H 0.435254 0.484926 0.682232 0.056 Uiso 1 1 calc R U . . .
C6 C 0.09593(18) 0.30728(17) 0.33893(17) 0.0282(7) Uani 1 1 d . . . . .
H6A H 0.130981 0.287580 0.312743 0.042 Uiso 1 1 calc R U . . .
H6B H 0.043994 0.289375 0.317396 0.042 Uiso 1 1 calc R U . . .
H6C H 0.111458 0.286785 0.385675 0.042 Uiso 1 1 calc R U . . .
C25 C 0.3825(2) 0.27337(18) 0.40435(19) 0.0341(8) Uani 1 1 d . . . . .
H25A H 0.419054 0.273767 0.449153 0.051 Uiso 1 1 calc R U . . .
H25B H 0.381064 0.220345 0.384190 0.051 Uiso 1 1 calc R U . . .
H25C H 0.331698 0.287212 0.409595 0.051 Uiso 1 1 calc R U . . .
C13 C 0.3035(2) 0.5488(2) 0.60537(17) 0.0322(7) Uani 1 1 d . . . . .
H13A H 0.346007 0.585959 0.609347 0.048 Uiso 1 1 calc R U . . .
H13B H 0.279849 0.556949 0.643498 0.048 Uiso 1 1 calc R U . . .
H13C H 0.265530 0.558037 0.562188 0.048 Uiso 1 1 calc R U . . .
C7 C 0.12139(17) 0.4238(2) 0.21773(15) 0.0274(7) Uani 1 1 d . . . . .
H7A H 0.152499 0.463302 0.201490 0.041 Uiso 1 1 calc R U . . .
H7B H 0.071851 0.418801 0.184622 0.041 Uiso 1 1 calc R U . . .
H7C H 0.147590 0.372440 0.222924 0.041 Uiso 1 1 calc R U . . .
C15 C 0.2661(2) 0.4024(2) 0.60019(18) 0.0370(8) Uani 1 1 d . . . . .
H15A H 0.228815 0.411222 0.556582 0.056 Uiso 1 1 calc R U . . .
H15B H 0.241723 0.410782 0.637768 0.056 Uiso 1 1 calc R U . . .
H15C H 0.285389 0.347881 0.601881 0.056 Uiso 1 1 calc R U . . .
C12 C 0.33386(18) 0.46170(18) 0.60711(16) 0.0250(7) Uani 1 1 d . . . . .
C8 C 0.10575(18) 0.60574(19) 0.26269(16) 0.0281(7) Uani 1 1 d . . . . .
H8A H 0.114303 0.653364 0.291370 0.042 Uiso 1 1 calc R U . . .
H8B H 0.057684 0.611132 0.227648 0.042 Uiso 1 1 calc R U . . .
H8C H 0.147919 0.599292 0.240715 0.042 Uiso 1 1 calc R U . . .
C18 C 0.4238(2) 0.75043(19) 0.42538(17) 0.0387(9) Uani 1 1 d . . . . .
H18A H 0.430554 0.761887 0.474014 0.058 Uiso 1 1 calc R U . . .
H18B H 0.408139 0.798888 0.398809 0.058 Uiso 1 1 calc R U . . .
H18C H 0.472006 0.731255 0.417535 0.058 Uiso 1 1 calc R U . . .
C24 C 0.3476(2) 0.3381(2) 0.28639(17) 0.0392(9) Uani 1 1 d . . . . .
H24A H 0.298867 0.357576 0.292981 0.059 Uiso 1 1 calc R U . . .
H24B H 0.340533 0.284712 0.266634 0.059 Uiso 1 1 calc R U . . .
H24C H 0.365519 0.373788 0.255457 0.059 Uiso 1 1 calc R U . . .
C19 C 0.3520(3) 0.6665(2) 0.32605(18) 0.0576(13) Uani 1 1 d . . . . .
H19A H 0.401003 0.648253 0.319214 0.086 Uiso 1 1 calc R U . . .
H19B H 0.335842 0.714389 0.298878 0.086 Uiso 1 1 calc R U . . .
H19C H 0.313591 0.624806 0.311650 0.086 Uiso 1 1 calc R U . . .
C20 C 0.2851(2) 0.7167(2) 0.4137(3) 0.0614(13) Uani 1 1 d . . . . .
H20A H 0.245103 0.676806 0.398449 0.092 Uiso 1 1 calc R U . . .
H20B H 0.270909 0.765640 0.387497 0.092 Uiso 1 1 calc R U . . .
H20C H 0.290977 0.727660 0.462349 0.092 Uiso 1 1 calc R U . . .
H H 0.246(3) 0.413(3) 0.426(3) 0.112(19) Uiso 1 1 d . . . . .
HA H 0.240(3) 0.545(3) 0.435(3) 0.080(15) Uiso 1 1 d . . . . .
HB H 0.263(5) 0.483(4) 0.345(4) 0.17(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 Ta1 2.48172(16) . ?
Os1 C1 2.233(3) . ?
Os1 C5 2.227(3) . ?
Os1 C4 2.223(3) . ?
Os1 C3 2.226(3) . ?
Os1 C2 2.235(3) . ?
Os1 H 1.45(5) . ?
Os1 HA 1.56(5) . ?
Os1 HB 1.48(8) . ?
Ta1 C21 2.132(3) . ?
Ta1 C16 2.136(3) . ?
Ta1 C11 2.143(3) . ?
Ta1 H 2.07(5) . ?
Ta1 HA 2.03(5) . ?
Ta1 HB 2.07(8) . ?
C17 C16 1.535(4) . ?
C17 C18 1.534(4) . ?
C17 C19 1.519(4) . ?
C17 C20 1.505(5) . ?
C1 C5 1.446(4) . ?
C1 C2 1.418(4) . ?
C1 C6 1.506(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.540(4) . ?
C5 C4 1.435(4) . ?
C5 C10 1.494(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.542(4) . ?
C22 C23 1.531(4) . ?
C22 C25 1.532(4) . ?
C22 C24 1.529(4) . ?
C4 C3 1.425(4) . ?
C4 C9 1.502(4) . ?
C3 C2 1.440(4) . ?
C3 C8 1.507(4) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C2 C7 1.497(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14 C12 1.536(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C13 C12 1.533(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 C12 1.529(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ta1 Os1 H 56(2) . . ?
Ta1 Os1 HA 54.7(17) . . ?
Ta1 Os1 HB 56(3) . . ?
C1 Os1 Ta1 148.77(7) . . ?
C1 Os1 C2 37.01(10) . . ?
C1 Os1 H 94(2) . . ?
C1 Os1 HA 148.4(18) . . ?
C1 Os1 HB 119(3) . . ?
C5 Os1 Ta1 146.85(7) . . ?
C5 Os1 C1 37.83(10) . . ?
C5 Os1 C2 62.60(10) . . ?
C5 Os1 H 100(2) . . ?
C5 Os1 HA 110.6(18) . . ?
C5 Os1 HB 155(3) . . ?
C4 Os1 Ta1 145.06(7) . . ?
C4 Os1 C1 62.79(10) . . ?
C4 Os1 C5 37.62(10) . . ?
C4 Os1 C3 37.36(11) . . ?
C4 Os1 C2 62.55(10) . . ?
C4 Os1 H 135(2) . . ?
C4 Os1 HA 90.3(17) . . ?
C4 Os1 HB 136(3) . . ?
C3 Os1 Ta1 145.48(7) . . ?
C3 Os1 C1 62.62(10) . . ?
C3 Os1 C5 62.80(10) . . ?
C3 Os1 C2 37.66(10) . . ?
C3 Os1 H 157(2) . . ?
C3 Os1 HA 106.6(17) . . ?
C3 Os1 HB 101(3) . . ?
C2 Os1 Ta1 147.97(8) . . ?
C2 Os1 H 122(2) . . ?
C2 Os1 HA 144.1(17) . . ?
C2 Os1 HB 93(3) . . ?
H Os1 HA 94(3) . . ?
H Os1 HB 89(3) . . ?
HA Os1 HB 92(3) . . ?
Os1 Ta1 H 35.8(15) . . ?
Os1 Ta1 HA 38.9(13) . . ?
Os1 Ta1 HB 37(2) . . ?
C21 Ta1 Os1 114.18(7) . . ?
C21 Ta1 C16 104.88(11) . . ?
C21 Ta1 C11 104.75(11) . . ?
C21 Ta1 H 101.4(16) . . ?
C21 Ta1 HA 149.2(14) . . ?
C21 Ta1 HB 85(2) . . ?
C16 Ta1 Os1 113.56(7) . . ?
C16 Ta1 C11 103.75(11) . . ?
C16 Ta1 H 147.3(15) . . ?
C16 Ta1 HA 82.7(13) . . ?
C16 Ta1 HB 103.3(19) . . ?
C11 Ta1 Os1 114.59(8) . . ?
C11 Ta1 H 87.9(15) . . ?
C11 Ta1 HA 102.2(14) . . ?
C11 Ta1 HB 148(2) . . ?
H Ta1 HA 65(2) . . ?
H Ta1 HB 60(2) . . ?
HA Ta1 HB 64(3) . . ?
C18 C17 C16 109.0(2) . . ?
C19 C17 C16 109.0(3) . . ?
C19 C17 C18 108.9(3) . . ?
C20 C17 C16 110.8(3) . . ?
C20 C17 C18 109.0(3) . . ?
C20 C17 C19 110.0(3) . . ?
C5 C1 Os1 70.86(14) . . ?
C5 C1 C6 125.4(3) . . ?
C2 C1 Os1 71.58(15) . . ?
C2 C1 C5 108.1(2) . . ?
C2 C1 C6 126.3(3) . . ?
C6 C1 Os1 126.8(2) . . ?
Ta1 C21 H21A 104.0 . . ?
Ta1 C21 H21B 104.0 . . ?
H21A C21 H21B 105.5 . . ?
C22 C21 Ta1 133.0(2) . . ?
C22 C21 H21A 104.0 . . ?
C22 C21 H21B 104.0 . . ?
C1 C5 Os1 71.31(15) . . ?
C1 C5 C10 126.6(2) . . ?
C4 C5 Os1 71.03(15) . . ?
C4 C5 C1 107.4(2) . . ?
C4 C5 C10 125.8(3) . . ?
C10 C5 Os1 127.18(19) . . ?
Ta1 C16 H16A 103.6 . . ?
Ta1 C16 H16B 103.6 . . ?
C17 C16 Ta1 134.21(19) . . ?
C17 C16 H16A 103.6 . . ?
C17 C16 H16B 103.6 . . ?
H16A C16 H16B 105.3 . . ?
Ta1 C11 H11A 104.5 . . ?
Ta1 C11 H11B 104.5 . . ?
H11A C11 H11B 105.7 . . ?
C12 C11 Ta1 130.9(2) . . ?
C12 C11 H11A 104.5 . . ?
C12 C11 H11B 104.5 . . ?
C23 C22 C21 109.5(2) . . ?
C23 C22 C25 108.8(2) . . ?
C25 C22 C21 109.4(2) . . ?
C24 C22 C21 110.3(2) . . ?
C24 C22 C23 109.0(3) . . ?
C24 C22 C25 109.8(3) . . ?
C5 C4 Os1 71.35(15) . . ?
C5 C4 C9 125.0(3) . . ?
C3 C4 Os1 71.43(16) . . ?
C3 C4 C5 108.4(2) . . ?
C3 C4 C9 126.6(2) . . ?
C9 C4 Os1 125.07(19) . . ?
C4 C3 Os1 71.21(15) . . ?
C4 C3 C2 107.8(2) . . ?
C4 C3 C8 127.3(3) . . ?
C2 C3 Os1 71.53(15) . . ?
C2 C3 C8 124.8(3) . . ?
C8 C3 Os1 125.7(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C1 C2 Os1 71.42(15) . . ?
C1 C2 C3 108.3(2) . . ?
C1 C2 C7 126.2(3) . . ?
C3 C2 Os1 70.81(15) . . ?
C3 C2 C7 125.3(3) . . ?
C7 C2 Os1 126.8(2) . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
C14 C12 C11 109.6(3) . . ?
C13 C12 C11 110.2(2) . . ?
C13 C12 C14 108.5(3) . . ?
C15 C12 C11 109.9(3) . . ?
C15 C12 C14 109.0(3) . . ?
C15 C12 C13 109.6(3) . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Os1 C1 C5 C4 62.26(18) . . . . ?
Os1 C1 C5 C10 -122.9(3) . . . . ?
Os1 C1 C2 C3 -61.52(19) . . . . ?
Os1 C1 C2 C7 122.5(3) . . . . ?
Os1 C5 C4 C3 62.18(19) . . . . ?
Os1 C5 C4 C9 -120.3(3) . . . . ?
Os1 C4 C3 C2 62.57(18) . . . . ?
Os1 C4 C3 C8 -121.0(3) . . . . ?
Os1 C3 C2 C1 61.91(19) . . . . ?
Os1 C3 C2 C7 -122.0(3) . . . . ?
Ta1 C21 C22 C23 -167.1(2) . . . . ?
Ta1 C21 C22 C25 -47.9(3) . . . . ?
Ta1 C21 C22 C24 73.0(4) . . . . ?
Ta1 C11 C12 C14 -160.3(2) . . . . ?
Ta1 C11 C12 C13 -41.0(4) . . . . ?
Ta1 C11 C12 C15 80.0(3) . . . . ?
C1 C5 C4 Os1 -62.45(18) . . . . ?
C1 C5 C4 C3 -0.3(3) . . . . ?
C1 C5 C4 C9 177.3(3) . . . . ?
C5 C1 C2 Os1 61.82(18) . . . . ?
C5 C1 C2 C3 0.3(3) . . . . ?
C5 C1 C2 C7 -175.7(3) . . . . ?
C5 C4 C3 Os1 -62.13(18) . . . . ?
C5 C4 C3 C2 0.4(3) . . . . ?
C5 C4 C3 C8 176.9(3) . . . . ?
C4 C3 C2 Os1 -62.37(19) . . . . ?
C4 C3 C2 C1 -0.5(3) . . . . ?
C4 C3 C2 C7 175.6(3) . . . . ?
C10 C5 C4 Os1 122.7(3) . . . . ?
C10 C5 C4 C3 -175.1(3) . . . . ?
C10 C5 C4 C9 2.4(4) . . . . ?
C2 C1 C5 Os1 -62.28(19) . . . . ?
C2 C1 C5 C4 0.0(3) . . . . ?
C2 C1 C5 C10 174.8(3) . . . . ?
C9 C4 C3 Os1 120.4(3) . . . . ?
C9 C4 C3 C2 -177.1(3) . . . . ?
C9 C4 C3 C8 -0.6(5) . . . . ?
C6 C1 C5 Os1 122.1(3) . . . . ?
C6 C1 C5 C4 -175.6(3) . . . . ?
C6 C1 C5 C10 -0.8(4) . . . . ?
C6 C1 C2 Os1 -122.7(3) . . . . ?
C6 C1 C2 C3 175.8(3) . . . . ?
C6 C1 C2 C7 -0.2(5) . . . . ?
C8 C3 C2 Os1 121.1(3) . . . . ?
C8 C3 C2 C1 -177.0(3) . . . . ?
C8 C3 C2 C7 -0.9(4) . . . . ?
C18 C17 C16 Ta1 -171.7(2) . . . . ?
C19 C17 C16 Ta1 -53.0(4) . . . . ?
C20 C17 C16 Ta1 68.3(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.653
_oxdiff_exptl_absorpt_empirical_full_min 0.593
####################################################################### 
# 
# 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_al143_2_autored
_database_code_depnum_ccdc_archive 'CCDC 2351850'
loop_
_audit_author_name
_audit_author_address
'Erwann Jeanneau'
;universite Claude Bernard Lyon
France
;
_audit_update_record             
;
2024-06-10 deposited with the CCDC.	2024-06-26 downloaded from the CCDC.
;
_audit_creation_date             2024-06-10
_audit_creation_method           
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H18 O Os'
_chemical_formula_sum            'C11 H18 O Os'
_chemical_formula_weight         356.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44 H60 O4 Os4 '
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   8.1490(2)
_cell_length_b                   11.0276(2)
_cell_length_c                   13.2481(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.769(2)
_cell_angle_gamma                90
_cell_volume                     1165.50(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20648
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      30.3780
_cell_measurement_theta_min      2.4220
_shelx_estimated_absorpt_T_max   0.230
_shelx_estimated_absorpt_T_min   0.157
_exptl_absorpt_coefficient_mu    10.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.031
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 1 0.0875
0 1 -1 0.1033
0 1 -2 0.1098
0 1 1 0.0991
0 -1 -1 0.1175
-1 2 -2 0.1040
1 -2 2 0.0961
0 2 1 0.1057
1 0 2 0.1020
1 -1 2 0.1044
0 -2 -1 0.1223
-1 0 -2 0.1054
-1 2 -1 0.1075
-1 -1 -2 0.1109
1 1 2 0.1066
-1 0 -1 0.1023
-2 2 -1 0.1083
-1 -2 -2 0.1162
1 0 1 0.0937
1 2 2 0.1169
2 0 1 0.0890
-2 0 -1 0.1053
-2 -2 -1 0.1077
-1 1 0 0.1218
-2 1 0 0.1248
-2 -1 0 0.1076
2 1 0 0.1223
-2 -2 1 0.1097
-2 1 1 0.1481
2 0 -1 0.1148
2 2 -1 0.1362
0 -1 0 0.1152
1 0 -1 0.1143
-1 2 1 0.1275
-1 -2 1 0.1004
-1 0 1 0.1574
1 1 -2 0.1201
-1 -2 2 0.1053
1 -1 -2 0.1301
-1 -6 17 0.1008
-3 6 17 0.1246

_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.191
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0012 -1.0003 0.9999 -0.0105 0.0620 -0.0563
0.0012 1.0003 -0.9999 0.0105 -0.0620 0.0563
0.0019 1.0011 -2.0001 0.0311 -0.1123 0.0502
-0.0001 0.9988 1.0006 -0.0307 0.0385 0.0685
0.0001 -0.9988 -1.0006 0.0307 -0.0385 -0.0685
-0.9972 2.0013 -2.0014 0.1073 -0.1104 0.1292
0.9972 -2.0013 2.0014 -0.1073 0.1104 -0.1292
0.0004 1.9984 1.0009 -0.0408 0.0268 0.1309
0.9982 -0.0022 2.0020 -0.1275 0.0869 -0.0044
0.9977 -1.0017 2.0017 -0.1174 0.0987 -0.0668
-0.0004 -1.9984 -1.0009 0.0408 -0.0268 -0.1309
-0.9982 0.0022 -2.0020 0.1275 -0.0869 0.0044
-0.9978 2.0005 -1.0011 0.0867 -0.0601 0.1353
-0.9988 -0.9974 -2.0023 0.1376 -0.0752 -0.0580
0.9988 0.9974 2.0023 -0.1376 0.0752 0.0580
-0.9989 0.0014 -1.0018 0.1069 -0.0367 0.0104
-1.9974 2.0012 -1.0027 0.1730 -0.0465 0.1518
-0.9993 -1.9970 -2.0027 0.1476 -0.0635 -0.1205
0.9989 -0.0014 1.0018 -0.1069 0.0367 -0.0104
0.9993 1.9970 2.0027 -0.1476 0.0635 0.1205
1.9985 -0.0021 1.0033 -0.1932 0.0230 -0.0270
-1.9985 0.0021 -1.0033 0.1932 -0.0230 0.0270
-1.9996 -1.9970 -1.0040 0.2133 0.0005 -0.0978
-0.9991 1.0002 -0.0012 0.0762 0.0019 0.0789
-1.9987 1.0009 -0.0028 0.1625 0.0155 0.0955
-1.9998 -0.9982 -0.0034 0.1827 0.0390 -0.0294
1.9998 0.9982 0.0034 -0.1827 -0.0390 0.0294
-2.0010 -1.9985 0.9965 0.1722 0.1010 -0.0857
-1.9994 1.0002 0.9974 0.1419 0.0658 0.1015
1.9999 -0.0006 -0.9971 -0.1520 -0.0776 -0.0391
2.0010 1.9985 -0.9965 -0.1722 -0.1010 0.0857
-0.0005 -0.9996 -0.0003 0.0101 0.0117 -0.0624
1.0003 0.0001 -0.9987 -0.0657 -0.0639 -0.0226
-0.9992 1.9991 0.9993 0.0455 0.0404 0.1474
-1.0014 -1.9992 0.9980 0.0859 0.0874 -0.1022
-1.0003 -0.0001 0.9987 0.0657 0.0639 0.0226
1.0015 1.0004 -1.9986 -0.0552 -0.1259 0.0337
-1.0021 -2.0000 1.9983 0.0653 0.1377 -0.0961
1.0004 -0.9987 -1.9992 -0.0350 -0.1025 -0.0911
-1.3697 -5.8593 17.2513 -0.1792 0.9547 -0.2377
-3.0266 6.0108 17.1687 -0.1537 0.8338 0.5303

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26457
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.382
_diffrn_reflns_theta_min         2.424
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -6.00  39.00   0.50    1.68    --    7.11  57.00-180.00   90
  2  ω    -19.00  39.00   0.50    1.68    --   -6.25  57.00-150.00  116
  3  ω     -6.00  39.00   0.50    1.68    --    7.11  57.00-120.00   90
  4  ω    -60.00   7.00   0.50    1.68    --   -6.25 -57.00 -90.00  134
  5  ω    -85.00 -40.00   0.50    1.68    --   -6.25 -19.00-150.00   90
  6  ω    -85.00 -44.00   0.50    1.68    --   -6.25 -18.00 -35.00   82
  7  ω      1.00  86.00   0.50    1.68    --    7.11  18.00 132.00  170
  8  ω      1.00  73.00   0.50    1.68    --   -6.25  18.00 132.00  144
  9  ω     -4.00  42.00   0.50    1.68    --    7.11 -99.00 -30.00   92
 10  ω     -4.00  42.00   0.50    1.68    --    7.11 -99.00-180.00   92
 11  ω     -4.00  42.00   0.50    1.68    --    7.11 -99.00  60.00   92
 12  ω     -4.00  42.00   0.50    1.68    --    7.11 -99.00 120.00   92
 13  ω    -73.00 -48.00   0.50    1.68    --    7.11 -19.00  60.00   50
 14  ω    -73.00 -40.00   0.50    1.68    --    7.11 -19.00  30.00   66
 15  ω    -72.00 -44.00   0.50    1.68    --    7.11 -18.00 -35.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0862945000
_diffrn_orient_matrix_UB_12      -0.0100409000
_diffrn_orient_matrix_UB_13      -0.0206514000
_diffrn_orient_matrix_UB_21      -0.0137231000
_diffrn_orient_matrix_UB_22      -0.0117520000
_diffrn_orient_matrix_UB_23      0.0502575000
_diffrn_orient_matrix_UB_31      -0.0165004000
_diffrn_orient_matrix_UB_32      0.0624391000
_diffrn_orient_matrix_UB_33      0.0061190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2903
_reflns_number_total             3126
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.105a 64-bit (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.410
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.00155(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         3126
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0212
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0232P)²+1.3111P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0503
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
HA \\sim HB \\sim HC: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.08 within 1.7A
3. Rigid body (RIGU) restrains
 C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Uiso: HA(0.035) HB(0.035) HC(0.035)
5.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.52658(2) 0.81359(2) 0.69177(2) 0.01391(6) Uani 1 1 d . . . . .
HA H 0.700(5) 0.774(4) 0.751(3) 0.035 Uiso 1 1 d . U . . .
HB H 0.679(5) 0.900(4) 0.687(3) 0.035 Uiso 1 1 d . U . . .
HC H 0.484(5) 0.946(4) 0.678(3) 0.035 Uiso 1 1 d . U . . .
O1 O 0.4742(3) 0.8745(2) 0.90463(17) 0.0282(5) Uani 1 1 d . . . . .
C1 C 0.4970(4) 0.8522(3) 0.8229(2) 0.0192(6) Uani 1 1 d . . . . .
C2 C 0.3256(4) 0.7893(3) 0.5453(2) 0.0146(5) Uani 1 1 d . . . . .
C3 C 0.2843(4) 0.7132(3) 0.6244(2) 0.0146(5) Uani 1 1 d . . . . .
C4 C 0.4193(4) 0.6272(2) 0.6545(2) 0.0131(5) Uani 1 1 d . . . . .
C5 C 0.5399(4) 0.6488(3) 0.5914(2) 0.0139(5) Uani 1 1 d . . . . .
C6 C 0.4836(4) 0.7497(2) 0.5247(2) 0.0147(5) Uani 1 1 d . . . . .
C7 C 0.2160(4) 0.8862(3) 0.4871(2) 0.0228(6) Uani 1 1 d . . . . .
H7A H 0.147042 0.922331 0.531778 0.034 Uiso 1 1 calc R U . . .
H7B H 0.143212 0.850588 0.426319 0.034 Uiso 1 1 calc R U . . .
H7C H 0.286333 0.949108 0.465231 0.034 Uiso 1 1 calc R U . . .
C8 C 0.1230(4) 0.7123(3) 0.6618(3) 0.0231(6) Uani 1 1 d . . . . .
H8A H 0.145011 0.690935 0.735096 0.035 Uiso 1 1 calc R U . . .
H8B H 0.046682 0.652542 0.622437 0.035 Uiso 1 1 calc R U . . .
H8C H 0.071490 0.792936 0.652231 0.035 Uiso 1 1 calc R U . . .
C9 C 0.4184(4) 0.5221(3) 0.7259(2) 0.0208(6) Uani 1 1 d . . . . .
H9A H 0.534011 0.499933 0.757279 0.031 Uiso 1 1 calc R U . . .
H9B H 0.362306 0.452900 0.687070 0.031 Uiso 1 1 calc R U . . .
H9C H 0.358337 0.544736 0.780074 0.031 Uiso 1 1 calc R U . . .
C10 C 0.6902(4) 0.5715(3) 0.5886(2) 0.0208(6) Uani 1 1 d . . . . .
H10A H 0.768962 0.616633 0.555959 0.031 Uiso 1 1 calc R U . . .
H10B H 0.654807 0.497628 0.548982 0.031 Uiso 1 1 calc R U . . .
H10C H 0.745166 0.549552 0.659128 0.031 Uiso 1 1 calc R U . . .
C11 C 0.5618(5) 0.7948(3) 0.4388(2) 0.0224(7) Uani 1 1 d . . . . .
H11A H 0.541368 0.882041 0.429466 0.034 Uiso 1 1 calc R U . . .
H11B H 0.512345 0.752143 0.374879 0.034 Uiso 1 1 calc R U . . .
H11C H 0.682789 0.779626 0.455713 0.034 Uiso 1 1 calc R U . . .


_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 HA 1.53(4) . ?
Os1 HB 1.58(4) . ?
Os1 HC 1.51(4) . ?
Os1 C1 1.851(3) . ?
Os1 C2 2.286(3) . ?
Os1 C3 2.280(3) . ?
Os1 C4 2.249(3) . ?
Os1 C5 2.267(3) . ?
Os1 C6 2.281(3) . ?
O1 C1 1.162(4) . ?
C2 C3 1.435(4) . ?
C2 C6 1.438(4) . ?
C2 C7 1.501(4) . ?
C3 C4 1.445(4) . ?
C3 C8 1.497(4) . ?
C4 C5 1.434(4) . ?
C4 C9 1.496(4) . ?
C5 C6 1.437(4) . ?
C5 C10 1.499(4) . ?
C6 C11 1.498(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
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 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
HA Os1 HB 63(2) . . ?
HA Os1 HC 120(2) . . ?
HB Os1 HC 65(2) . . ?
C1 Os1 HA 82.2(15) . . ?
C1 Os1 HB 99.0(15) . . ?
C1 Os1 HC 79.8(15) . . ?
C1 Os1 C2 128.00(12) . . ?
C1 Os1 C3 102.17(12) . . ?
C1 Os1 C4 107.27(12) . . ?
C1 Os1 C5 139.95(12) . . ?
C1 Os1 C6 163.33(12) . . ?
C2 Os1 HA 146.0(15) . . ?
C2 Os1 HB 117.9(15) . . ?
C2 Os1 HC 84.3(16) . . ?
C3 Os1 HA 134.2(16) . . ?
C3 Os1 HB 154.4(15) . . ?
C3 Os1 HC 105.2(17) . . ?
C3 Os1 C2 36.65(10) . . ?
C3 Os1 C6 61.38(10) . . ?
C4 Os1 HA 97.5(16) . . ?
C4 Os1 HB 144.8(15) . . ?
C4 Os1 HC 142.2(17) . . ?
C4 Os1 C2 61.80(10) . . ?
C4 Os1 C3 37.21(10) . . ?
C4 Os1 C5 37.03(10) . . ?
C4 Os1 C6 61.89(10) . . ?
C5 Os1 HA 85.7(15) . . ?
C5 Os1 HB 109.1(15) . . ?
C5 Os1 HC 137.9(15) . . ?
C5 Os1 C2 61.32(10) . . ?
C5 Os1 C3 61.49(10) . . ?
C5 Os1 C6 36.84(10) . . ?
C6 Os1 HA 110.8(15) . . ?
C6 Os1 HB 96.4(15) . . ?
C6 Os1 HC 101.1(15) . . ?
C6 Os1 C2 36.70(10) . . ?
O1 C1 Os1 178.0(3) . . ?
C3 C2 Os1 71.47(16) . . ?
C3 C2 C6 108.2(2) . . ?
C3 C2 C7 126.0(3) . . ?
C6 C2 Os1 71.47(16) . . ?
C6 C2 C7 125.5(3) . . ?
C7 C2 Os1 126.9(2) . . ?
C2 C3 Os1 71.88(16) . . ?
C2 C3 C4 107.9(2) . . ?
C2 C3 C8 126.7(3) . . ?
C4 C3 Os1 70.21(15) . . ?
C4 C3 C8 125.1(3) . . ?
C8 C3 Os1 128.5(2) . . ?
C3 C4 Os1 72.58(15) . . ?
C3 C4 C9 125.5(3) . . ?
C5 C4 Os1 72.16(15) . . ?
C5 C4 C3 107.7(2) . . ?
C5 C4 C9 126.1(3) . . ?
C9 C4 Os1 128.37(19) . . ?
C4 C5 Os1 70.80(15) . . ?
C4 C5 C6 108.5(2) . . ?
C4 C5 C10 125.5(3) . . ?
C6 C5 Os1 72.11(16) . . ?
C6 C5 C10 125.8(3) . . ?
C10 C5 Os1 127.4(2) . . ?
C2 C6 Os1 71.83(16) . . ?
C2 C6 C11 125.4(3) . . ?
C5 C6 Os1 71.04(16) . . ?
C5 C6 C2 107.7(2) . . ?
C5 C6 C11 126.3(3) . . ?
C11 C6 Os1 129.1(2) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Os1 C2 C3 C4 -61.32(18) . . . . ?
Os1 C2 C3 C8 125.0(3) . . . . ?
Os1 C2 C6 C5 62.36(19) . . . . ?
Os1 C2 C6 C11 -125.5(3) . . . . ?
Os1 C3 C4 C5 -64.10(18) . . . . ?
Os1 C3 C4 C9 125.1(3) . . . . ?
Os1 C4 C5 C6 -62.68(19) . . . . ?
Os1 C4 C5 C10 122.8(3) . . . . ?
Os1 C5 C6 C2 -62.87(19) . . . . ?
Os1 C5 C6 C11 125.1(3) . . . . ?
C2 C3 C4 Os1 62.39(19) . . . . ?
C2 C3 C4 C5 -1.7(3) . . . . ?
C2 C3 C4 C9 -172.5(3) . . . . ?
C3 C2 C6 Os1 -62.40(19) . . . . ?
C3 C2 C6 C5 0.0(3) . . . . ?
C3 C2 C6 C11 172.1(3) . . . . ?
C3 C4 C5 Os1 64.37(18) . . . . ?
C3 C4 C5 C6 1.7(3) . . . . ?
C3 C4 C5 C10 -172.8(3) . . . . ?
C4 C5 C6 Os1 61.84(19) . . . . ?
C4 C5 C6 C2 -1.0(3) . . . . ?
C4 C5 C6 C11 -173.1(3) . . . . ?
C6 C2 C3 Os1 62.40(19) . . . . ?
C6 C2 C3 C4 1.1(3) . . . . ?
C6 C2 C3 C8 -172.6(3) . . . . ?
C7 C2 C3 Os1 -122.7(3) . . . . ?
C7 C2 C3 C4 176.0(3) . . . . ?
C7 C2 C3 C8 2.3(5) . . . . ?
C7 C2 C6 Os1 122.6(3) . . . . ?
C7 C2 C6 C5 -175.0(3) . . . . ?
C7 C2 C6 C11 -2.8(5) . . . . ?
C8 C3 C4 Os1 -123.8(3) . . . . ?
C8 C3 C4 C5 172.1(3) . . . . ?
C8 C3 C4 C9 1.3(4) . . . . ?
C9 C4 C5 Os1 -124.9(3) . . . . ?
C9 C4 C5 C6 172.4(3) . . . . ?
C9 C4 C5 C10 -2.1(4) . . . . ?
C10 C5 C6 Os1 -123.7(3) . . . . ?
C10 C5 C6 C2 173.4(3) . . . . ?
C10 C5 C6 C11 1.4(5) . . . . ?

_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id AL143_2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.402
_oxdiff_exptl_absorpt_empirical_full_min 0.724
