# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_C32H36Os
_database_code_depnum_ccdc_archive 'CCDC 2024175'
loop_
_audit_author_name
_audit_author_address
'Ralf Haiges'
;University of Southern California
United States of America
;
_audit_update_record             
;
2020-08-19 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_chemical_name_systematic        tetrakis(2,5-dimethylphenyl)osmium(IV)
_chemical_name_common            Os(2,5-xylyl)4
_chemical_formula_moiety         'C32 H36 Os'
_chemical_formula_sum            'C32 H36 Os'
_chemical_formula_iupac          ?
_chemical_formula_weight         610.81
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 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'

_cell_length_a                   12.9059(19)
_cell_length_b                   12.9355(18)
_cell_length_c                   15.837(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.736(2)
_cell_angle_gamma                90
_cell_volume                     2613.2(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9989
_cell_measurement_theta_min      2.4679
_cell_measurement_theta_max      30.5925
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.022
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216

_exptl_absorpt_coefficient_mu    4.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_T_max  0.90

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            32067
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_full        30.52
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22

_refine_special_details          
;
;

_reflns_number_total             7862
_reflns_number_gt                7265
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_gt          0.0406
_refine_ls_wR_factor_ref         0.0416
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_restrained_S_all      0.952
_refine_ls_number_reflns         7862
_refine_ls_number_parameters     306
_refine_ls_number_restraints     2
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0012P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.535
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;

Flack x determined using 3368 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(6)

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'

_computing_data_collection       
'Bruker Instrument Service v2013.12.0.0 (Bruker AXS, 2013)'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2018/3 (Bruker AXS, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  'SHELXTL XL 2018/3 (Bruker AXS, 2018)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.2914(3) 0.7985(3) 0.4274(3) 0.0125(8) Uani d . . . 1 . .
C C2 0.3688(4) 0.8128(4) 0.3742(3) 0.0130(9) Uani d . . . 1 . .
C C3 0.3770(4) 0.9086(3) 0.3355(3) 0.0169(9) Uani d . . . 1 . .
H H3 0.430048 0.918797 0.300799 0.02 Uiso calc U . R 1 . .
C C4 0.3096(3) 0.9895(3) 0.3465(3) 0.0173(9) Uani d . . . 1 . .
H H4 0.318556 1.054639 0.320865 0.021 Uiso calc U . R 1 . .
C C5 0.2288(3) 0.9759(3) 0.3951(3) 0.0162(9) Uani d . . . 1 . .
C C6 0.2208(3) 0.8812(3) 0.4337(3) 0.0140(9) Uani d . . . 1 . .
H H6 0.165349 0.870998 0.466081 0.017 Uiso calc U . R 1 . .
C C7 0.4414(4) 0.7266(4) 0.3578(3) 0.0196(10) Uani d . . . 1 . .
H H7A 0.408996 0.685833 0.308661 0.029 Uiso calc U . R 1 . .
H H7B 0.45486 0.681988 0.408342 0.029 Uiso calc U . R 1 . .
H H7C 0.50775 0.755747 0.345846 0.029 Uiso calc U . R 1 . .
C C8 0.1540(6) 1.0632(5) 0.4086(5) 0.0243(16) Uani d . . . 1 . .
H H8A 0.160182 1.118725 0.367542 0.037 Uiso calc U . R 1 . .
H H8B 0.171633 1.090035 0.466821 0.037 Uiso calc U . R 1 . .
H H8C 0.08191 1.036938 0.39997 0.037 Uiso calc U . R 1 . .
C C9 0.4237(3) 0.6665(3) 0.5825(3) 0.0127(8) Uani d . . . 1 . .
C C10 0.4431(4) 0.5895(4) 0.6470(4) 0.0135(11) Uani d . . . 1 . .
C C11 0.5387(4) 0.5898(3) 0.6995(3) 0.0191(10) Uani d . . . 1 . .
H H11 0.552228 0.538811 0.742949 0.023 Uiso calc U . R 1 . .
C C12 0.6160(4) 0.6623(4) 0.6908(3) 0.0251(11) Uani d . . . 1 . .
H H12 0.68149 0.659313 0.727342 0.03 Uiso calc U . R 1 . .
C C13 0.5979(4) 0.7387(4) 0.6291(3) 0.0207(10) Uani d . . . 1 . .
C C14 0.5021(3) 0.7405(3) 0.5761(3) 0.0151(9) Uani d . . . 1 . .
H H14 0.488824 0.793282 0.534137 0.018 Uiso calc U . R 1 . .
C C15 0.3627(4) 0.5084(4) 0.6594(4) 0.0175(11) Uani d . . . 1 . .
H H15A 0.293053 0.531886 0.633138 0.026 Uiso calc U . R 1 . .
H H15B 0.363103 0.49688 0.720613 0.026 Uiso calc U . R 1 . .
H H15C 0.379816 0.443625 0.632471 0.026 Uiso calc U . R 1 . .
C C16 0.6815(5) 0.8194(4) 0.6193(5) 0.0339(16) Uani d . . . 1 . .
H H16A 0.71004 0.806428 0.566407 0.051 Uiso calc U . R 1 . .
H H16B 0.73796 0.814954 0.668133 0.051 Uiso calc U . R 1 . .
H H16C 0.650167 0.888497 0.617238 0.051 Uiso calc U . R 1 . .
C C17 0.1690(3) 0.6856(3) 0.5672(3) 0.0119(8) Uani d . . . 1 . .
C C18 0.1617(4) 0.7696(4) 0.6234(3) 0.0123(8) Uani d . . . 1 . .
C C19 0.0703(4) 0.7786(4) 0.6601(3) 0.0179(9) Uani d . . . 1 . .
H H19 0.06297 0.836091 0.696056 0.022 Uiso calc U . R 1 . .
C C20 -0.0106(3) 0.7064(3) 0.6458(3) 0.0151(9) Uani d . . . 1 . .
H H20 -0.072514 0.716125 0.670534 0.018 Uiso calc U . R 1 . .
C C21 -0.0005(3) 0.6200(3) 0.5954(3) 0.0149(9) Uani d . . . 1 . .
C C22 0.0885(3) 0.6109(3) 0.5564(3) 0.0137(8) Uani d . . . 1 . .
H H22 0.095286 0.552532 0.521288 0.016 Uiso calc U . R 1 . .
C C23 0.2495(4) 0.8454(3) 0.6468(3) 0.0182(10) Uani d . . . 1 . .
H H23A 0.284266 0.85829 0.596927 0.027 Uiso calc U . R 1 . .
H H23B 0.300268 0.816923 0.693265 0.027 Uiso calc U . R 1 . .
H H23C 0.221257 0.910442 0.665423 0.027 Uiso calc U . R 1 . .
C C24 -0.0844(6) 0.5363(5) 0.5849(5) 0.0232(16) Uani d . . . 1 . .
H H24A -0.151558 0.566158 0.593994 0.035 Uiso calc U . R 1 . .
H H24B -0.064489 0.481248 0.626742 0.035 Uiso calc U . R 1 . .
H H24C -0.091087 0.507462 0.527045 0.035 Uiso calc U . R 1 . .
C C25 0.2712(3) 0.5462(3) 0.4256(3) 0.0128(8) Uani d . . . 1 . .
C C26 0.1848(4) 0.5330(4) 0.3596(3) 0.0131(10) Uani d . . . 1 . .
C C27 0.1781(3) 0.4413(3) 0.3131(3) 0.0168(9) Uani d . . . 1 . .
H H27 0.121055 0.431562 0.268287 0.02 Uiso calc U . R 1 . .
C C28 0.2534(4) 0.3631(4) 0.3307(3) 0.0195(10) Uani d . . . 1 . .
H H28 0.245325 0.300358 0.299312 0.023 Uiso calc U . R 1 . .
C C29 0.3391(4) 0.3765(3) 0.3934(3) 0.0173(9) Uani d . . . 1 . .
C C30 0.3471(3) 0.4681(3) 0.4395(3) 0.0139(8) Uani d . . . 1 . .
H H30 0.406413 0.478318 0.482231 0.017 Uiso calc U . R 1 . .
C C31 0.1013(4) 0.6143(5) 0.3380(4) 0.0198(13) Uani d . . . 1 . .
H H31A 0.069511 0.607086 0.278008 0.03 Uiso calc U . R 1 . .
H H31B 0.132754 0.683105 0.347163 0.03 Uiso calc U . R 1 . .
H H31C 0.047229 0.605544 0.374687 0.03 Uiso calc U . R 1 . .
C C32 0.4230(5) 0.2945(4) 0.4087(4) 0.0249(12) Uani d . . . 1 . .
H H32A 0.468039 0.298862 0.364222 0.037 Uiso calc U . R 1 . .
H H32B 0.390177 0.226047 0.406937 0.037 Uiso calc U . R 1 . .
H H32C 0.46537 0.305266 0.464784 0.037 Uiso calc U . R 1 . .
Os Os1 0.28822(2) 0.67229(2) 0.50020(2) 0.00989(4) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.414(6) ?
C1 C6 . 1.419(6) ?
C1 Os1 . 2.003(4) ?
C2 C3 . 1.394(6) ?
C2 C7 . 1.504(7) ?
C3 C4 . 1.389(6) ?
C3 H3 . 0.95 ?
C4 C5 . 1.397(6) ?
C4 H4 . 0.95 ?
C5 C6 . 1.380(6) ?
C5 C8 . 1.521(8) ?
C6 H6 . 0.95 ?
C7 H7A . 0.98 ?
C7 H7B . 0.98 ?
C7 H7C . 0.98 ?
C8 H8A . 0.98 ?
C8 H8B . 0.98 ?
C8 H8C . 0.98 ?
C9 C14 . 1.407(6) ?
C9 C10 . 1.422(7) ?
C9 Os1 . 2.017(4) ?
C10 C11 . 1.379(6) ?
C10 C15 . 1.509(7) ?
C11 C12 . 1.391(7) ?
C11 H11 . 0.95 ?
C12 C13 . 1.385(7) ?
C12 H12 . 0.95 ?
C13 C14 . 1.385(6) ?
C13 C16 . 1.526(7) ?
C14 H14 . 0.95 ?
C15 H15A . 0.98 ?
C15 H15B . 0.98 ?
C15 H15C . 0.98 ?
C16 H16A . 0.98 ?
C16 H16B . 0.98 ?
C16 H16C . 0.98 ?
C17 C22 . 1.410(6) ?
C17 C18 . 1.418(6) ?
C17 Os1 . 2.005(4) ?
C18 C19 . 1.396(7) ?
C18 C23 . 1.501(7) ?
C19 C20 . 1.394(6) ?
C19 H19 . 0.95 ?
C20 C21 . 1.391(6) ?
C20 H20 . 0.95 ?
C21 C22 . 1.389(6) ?
C21 C24 . 1.522(8) ?
C22 H22 . 0.95 ?
C23 H23A . 0.98 ?
C23 H23B . 0.98 ?
C23 H23C . 0.98 ?
C24 H24A . 0.98 ?
C24 H24B . 0.98 ?
C24 H24C . 0.98 ?
C25 C30 . 1.401(6) ?
C25 C26 . 1.417(7) ?
C25 Os1 . 2.007(4) ?
C26 C27 . 1.392(6) ?
C26 C31 . 1.508(7) ?
C27 C28 . 1.401(6) ?
C27 H27 . 0.95 ?
C28 C29 . 1.380(6) ?
C28 H28 . 0.95 ?
C29 C30 . 1.389(6) ?
C29 C32 . 1.509(7) ?
C30 H30 . 0.95 ?
C31 H31A . 0.98 ?
C31 H31B . 0.98 ?
C31 H31C . 0.98 ?
C32 H32A . 0.98 ?
C32 H32B . 0.98 ?
C32 H32C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C6 . . 117.6(4) ?
C2 C1 Os1 . . 121.8(4) ?
C6 C1 Os1 . . 120.3(3) ?
C3 C2 C1 . . 119.1(5) ?
C3 C2 C7 . . 119.5(4) ?
C1 C2 C7 . . 121.4(4) ?
C4 C3 C2 . . 121.6(4) ?
C4 C3 H3 . . 119.2 ?
C2 C3 H3 . . 119.2 ?
C3 C4 C5 . . 120.5(4) ?
C3 C4 H4 . . 119.7 ?
C5 C4 H4 . . 119.7 ?
C6 C5 C4 . . 117.9(4) ?
C6 C5 C8 . . 120.2(5) ?
C4 C5 C8 . . 121.8(5) ?
C5 C6 C1 . . 123.0(4) ?
C5 C6 H6 . . 118.5 ?
C1 C6 H6 . . 118.5 ?
C2 C7 H7A . . 109.5 ?
C2 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C2 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C5 C8 H8A . . 109.5 ?
C5 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C5 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C14 C9 C10 . . 118.6(4) ?
C14 C9 Os1 . . 119.3(3) ?
C10 C9 Os1 . . 122.1(3) ?
C11 C10 C9 . . 118.3(5) ?
C11 C10 C15 . . 119.6(5) ?
C9 C10 C15 . . 122.1(4) ?
C10 C11 C12 . . 122.1(5) ?
C10 C11 H11 . . 118.9 ?
C12 C11 H11 . . 118.9 ?
C13 C12 C11 . . 120.3(4) ?
C13 C12 H12 . . 119.9 ?
C11 C12 H12 . . 119.9 ?
C12 C13 C14 . . 118.6(4) ?
C12 C13 C16 . . 120.9(5) ?
C14 C13 C16 . . 120.5(5) ?
C13 C14 C9 . . 122.0(4) ?
C13 C14 H14 . . 119.0 ?
C9 C14 H14 . . 119.0 ?
C10 C15 H15A . . 109.5 ?
C10 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C10 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
C13 C16 H16A . . 109.5 ?
C13 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C13 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C22 C17 C18 . . 118.9(4) ?
C22 C17 Os1 . . 119.2(3) ?
C18 C17 Os1 . . 121.9(3) ?
C19 C18 C17 . . 117.8(5) ?
C19 C18 C23 . . 119.8(4) ?
C17 C18 C23 . . 122.4(4) ?
C20 C19 C18 . . 122.4(4) ?
C20 C19 H19 . . 118.8 ?
C18 C19 H19 . . 118.8 ?
C21 C20 C19 . . 119.9(4) ?
C21 C20 H20 . . 120.0 ?
C19 C20 H20 . . 120.0 ?
C22 C21 C20 . . 118.6(4) ?
C22 C21 C24 . . 120.9(5) ?
C20 C21 C24 . . 120.5(5) ?
C21 C22 C17 . . 122.2(4) ?
C21 C22 H22 . . 118.9 ?
C17 C22 H22 . . 118.9 ?
C18 C23 H23A . . 109.5 ?
C18 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C18 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C21 C24 H24A . . 109.5 ?
C21 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C21 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
C30 C25 C26 . . 118.9(4) ?
C30 C25 Os1 . . 118.8(3) ?
C26 C25 Os1 . . 122.4(3) ?
C27 C26 C25 . . 118.1(5) ?
C27 C26 C31 . . 119.2(5) ?
C25 C26 C31 . . 122.6(5) ?
C26 C27 C28 . . 121.6(4) ?
C26 C27 H27 . . 119.2 ?
C28 C27 H27 . . 119.2 ?
C29 C28 C27 . . 120.6(4) ?
C29 C28 H28 . . 119.7 ?
C27 C28 H28 . . 119.7 ?
C28 C29 C30 . . 118.2(4) ?
C28 C29 C32 . . 120.3(4) ?
C30 C29 C32 . . 121.4(5) ?
C29 C30 C25 . . 122.5(4) ?
C29 C30 H30 . . 118.7 ?
C25 C30 H30 . . 118.7 ?
C26 C31 H31A . . 109.5 ?
C26 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C26 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C29 C32 H32A . . 109.5 ?
C29 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C29 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
C1 Os1 C17 . . 108.63(17) ?
C1 Os1 C25 . . 109.48(17) ?
C17 Os1 C25 . . 110.93(17) ?
C1 Os1 C9 . . 108.12(17) ?
C17 Os1 C9 . . 108.71(17) ?
C25 Os1 C9 . . 110.90(17) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . 4.4(6) ?
Os1 C1 C2 C3 . . . . -170.0(4) ?
C6 C1 C2 C7 . . . . -175.0(4) ?
Os1 C1 C2 C7 . . . . 10.6(6) ?
C1 C2 C3 C4 . . . . -1.4(7) ?
C7 C2 C3 C4 . . . . 178.0(4) ?
C2 C3 C4 C5 . . . . -2.0(7) ?
C3 C4 C5 C6 . . . . 2.2(6) ?
C3 C4 C5 C8 . . . . 179.8(5) ?
C4 C5 C6 C1 . . . . 1.0(6) ?
C8 C5 C6 C1 . . . . -176.6(5) ?
C2 C1 C6 C5 . . . . -4.3(6) ?
Os1 C1 C6 C5 . . . . 170.2(3) ?
C14 C9 C10 C11 . . . . -1.2(7) ?
Os1 C9 C10 C11 . . . . 178.6(4) ?
C14 C9 C10 C15 . . . . 178.9(5) ?
Os1 C9 C10 C15 . . . . -1.2(7) ?
C9 C10 C11 C12 . . . . -0.3(8) ?
C15 C10 C11 C12 . . . . 179.6(5) ?
C10 C11 C12 C13 . . . . 1.2(8) ?
C11 C12 C13 C14 . . . . -0.7(8) ?
C11 C12 C13 C16 . . . . 179.4(5) ?
C12 C13 C14 C9 . . . . -0.8(7) ?
C16 C13 C14 C9 . . . . 179.1(5) ?
C10 C9 C14 C13 . . . . 1.8(7) ?
Os1 C9 C14 C13 . . . . -178.1(4) ?
C22 C17 C18 C19 . . . . -5.1(6) ?
Os1 C17 C18 C19 . . . . 173.0(3) ?
C22 C17 C18 C23 . . . . 172.5(4) ?
Os1 C17 C18 C23 . . . . -9.4(6) ?
C17 C18 C19 C20 . . . . 2.5(7) ?
C23 C18 C19 C20 . . . . -175.1(4) ?
C18 C19 C20 C21 . . . . 1.9(7) ?
C19 C20 C21 C22 . . . . -3.5(7) ?
C19 C20 C21 C24 . . . . 175.3(5) ?
C20 C21 C22 C17 . . . . 0.8(6) ?
C24 C21 C22 C17 . . . . -177.9(5) ?
C18 C17 C22 C21 . . . . 3.5(6) ?
Os1 C17 C22 C21 . . . . -174.6(3) ?
C30 C25 C26 C27 . . . . 1.7(7) ?
Os1 C25 C26 C27 . . . . -177.9(3) ?
C30 C25 C26 C31 . . . . -177.9(5) ?
Os1 C25 C26 C31 . . . . 2.5(7) ?
C25 C26 C27 C28 . . . . 0.6(7) ?
C31 C26 C27 C28 . . . . -179.8(5) ?
C26 C27 C28 C29 . . . . -2.3(7) ?
C27 C28 C29 C30 . . . . 1.5(7) ?
C27 C28 C29 C32 . . . . -176.5(5) ?
C28 C29 C30 C25 . . . . 0.9(7) ?
C32 C29 C30 C25 . . . . 178.9(4) ?
C26 C25 C30 C29 . . . . -2.5(7) ?
Os1 C25 C30 C29 . . . . 177.1(3) ?



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

data_C32H36Os_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2175533'
loop_
_audit_author_name
_audit_author_address
'Thomas Saal'
;University of Southern California
United States of America
;
_audit_update_record             
;
2022-05-28 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_audit_creation_date             2022-05-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            Os1-Et
_chemical_name_systematic        tetrakis(2-ethylphenyl)osmium(IV)
_chemical_formula_moiety         'C32 H36 Os'
_chemical_formula_sum            'C32 H36 Os'
_chemical_formula_weight         610.81
_chemical_melting_point          ?
_chemical_oxdiff_formula         OsC12H24
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'

_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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   15.7666(3)
_cell_length_b                   15.7666(3)
_cell_length_c                   10.3145(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2564.04(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7582
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      33.4340
_cell_measurement_theta_min      3.4770
_shelx_estimated_absorpt_T_max   0.610
_shelx_estimated_absorpt_T_min   0.380
_exptl_absorpt_coefficient_mu    4.991
_exptl_absorpt_correction_T_max  0.419
_exptl_absorpt_correction_T_min  0.134
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.53a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -1 0 0.0416
-2 1 0 0.0713
1 -1 2 0.0996
0 1 0 0.0565
0 -1 0 0.0642
-2 -1 1 0.0886
2 1 -1 0.0939
-2 -2 1 0.0832
2 2 -1 0.0849
-1 -2 -1 0.1094
0 1 2 0.1021
-1 0 0 0.0656
-2 1 -2 0.1048
1 -1 -1 0.0967
-1 1 1 0.0715
2 2 1 0.0991
1 0 0 0.0679

_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.113
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
1.9965 -0.9976 -0.0004 -0.0633 0.0713 0.0315
-1.9965 0.9976 0.0004 0.0633 -0.0713 -0.0315
0.9978 -0.9990 1.9972 -0.0938 0.0493 -0.1080
0.0000 0.9984 0.0001 0.0414 0.0134 -0.0112
-0.0000 -0.9984 -0.0001 -0.0414 -0.0134 0.0112
-1.9968 -0.9997 0.9990 -0.0402 -0.0879 -0.0739
1.9968 0.9997 -0.9990 0.0402 0.0879 0.0739
-1.9968 -1.9982 0.9989 -0.0816 -0.1013 -0.0627
1.9968 1.9982 -0.9989 0.0816 0.1013 0.0627
-0.9981 -1.9968 -0.9987 -0.0511 -0.0793 0.0769
-0.0004 0.9974 1.9975 -0.0001 0.0338 -0.1406
-0.9983 -0.0004 0.0002 0.0109 -0.0424 -0.0102
-1.9961 0.9986 -1.9971 0.1047 -0.0917 0.0978
0.9984 -0.9975 -0.9989 -0.0316 0.0188 0.0860
-0.9984 0.9975 0.9989 0.0316 -0.0188 -0.0860
1.9964 1.9972 0.9985 0.0402 0.1217 -0.0667
0.9983 0.0004 -0.0002 -0.0109 0.0424 0.0102

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10077
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.857
_diffrn_reflns_theta_min         2.360
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_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 0.886
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -7.00  22.00   0.50    1.10    --   -9.49 -99.00   0.00   58
  2  ω     -7.00  22.00   0.50    1.10    --   -9.49 -99.00 120.00   58
  3  ω    -61.00 -27.00   0.50    1.10    --   10.12 -38.00  60.00   68
  4  ω    -25.00  11.00   0.50    1.10    --   -9.49 -77.00   0.00   72
  5  ω    -17.00  64.00   0.50    1.10    --   -9.49  26.00-125.00  162
;
_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      -0.0109823000
_diffrn_orient_matrix_UB_12      0.0414512000
_diffrn_orient_matrix_UB_13      -0.0207256000
_diffrn_orient_matrix_UB_21      0.0424218000
_diffrn_orient_matrix_UB_22      0.0134136000
_diffrn_orient_matrix_UB_23      0.0102135000
_diffrn_orient_matrix_UB_31      0.0101891000
_diffrn_orient_matrix_UB_32      -0.0111916000
_diffrn_orient_matrix_UB_33      -0.0647757000
_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                1863
_reflns_number_total             2114
_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 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.53a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         2114
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0185
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0097P)²+4.2545P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0396
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_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 0.500000 0.750000 0.125000 0.01003(4) Uani 1 4 d S T P . .
C1 C 0.56723(12) 0.82481(11) 0.24401(16) 0.0119(3) Uani 1 1 d . . . . .
C6 C 0.52645(12) 0.87302(12) 0.34192(16) 0.0131(3) Uani 1 1 d . . . . .
C2 C 0.65635(12) 0.82367(12) 0.23942(17) 0.0147(3) Uani 1 1 d . . . . .
H2 H 0.684110 0.791739 0.173856 0.018 Uiso 1 1 calc R U . . .
C7 C 0.43091(12) 0.87769(13) 0.35183(17) 0.0155(4) Uani 1 1 d . . . . .
H7A H 0.405782 0.847292 0.277142 0.019 Uiso 1 1 calc R U . . .
H7B H 0.413266 0.937830 0.345972 0.019 Uiso 1 1 calc R U . . .
C5 C 0.57687(13) 0.91664(12) 0.43159(18) 0.0163(4) Uani 1 1 d . . . . .
H5 H 0.550040 0.948637 0.497986 0.020 Uiso 1 1 calc R U . . .
C8 C 0.39544(14) 0.83983(15) 0.47719(19) 0.0234(4) Uani 1 1 d . . . . .
H8A H 0.333514 0.845124 0.477463 0.035 Uiso 1 1 calc R U . . .
H8B H 0.418984 0.870337 0.551748 0.035 Uiso 1 1 calc R U . . .
H8C H 0.411121 0.779793 0.482664 0.035 Uiso 1 1 calc R U . . .
C3 C 0.70465(13) 0.86854(13) 0.32933(18) 0.0175(4) Uani 1 1 d . . . . .
H3 H 0.764807 0.867684 0.324279 0.021 Uiso 1 1 calc R U . . .
C4 C 0.66443(13) 0.91461(13) 0.42654(19) 0.0185(4) Uani 1 1 d . . . . .
H4 H 0.696978 0.944525 0.489124 0.022 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 C1 2.0054(18) . ?
Os1 C1 2.0054(18) 6_564 ?
Os1 C1 2.0054(18) 12_766 ?
Os1 C1 2.0054(18) 15_565 ?
C1 C6 1.418(2) . ?
C1 C2 1.406(3) . ?
C6 C7 1.512(3) . ?
C6 C5 1.400(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.393(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.530(3) . ?
C5 H5 0.9500 . ?
C5 C4 1.382(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C3 H3 0.9500 . ?
C3 C4 1.391(3) . ?
C4 H4 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Os1 C1 112.00(5) . 12_766 ?
C1 Os1 C1 112.00(5) 12_766 6_564 ?
C1 Os1 C1 104.52(10) 12_766 15_565 ?
C1 Os1 C1 112.00(5) 15_565 6_564 ?
C1 Os1 C1 104.52(10) . 6_564 ?
C1 Os1 C1 112.00(5) . 15_565 ?
C6 C1 Os1 120.77(14) . . ?
C2 C1 Os1 120.01(13) . . ?
C2 C1 C6 118.94(17) . . ?
C1 C6 C7 121.74(16) . . ?
C5 C6 C1 118.44(18) . . ?
C5 C6 C7 119.81(17) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.16(18) . . ?
C3 C2 H2 119.4 . . ?
C6 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
C6 C7 C8 113.72(16) . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
C6 C5 H5 119.0 . . ?
C4 C5 C6 122.07(18) . . ?
C4 C5 H5 119.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.72(19) . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 119.65(18) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?

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 C6 C7 -6.7(2) . . . . ?
Os1 C1 C6 C5 172.88(14) . . . . ?
Os1 C1 C2 C3 -173.60(14) . . . . ?
C1 C6 C7 C8 116.5(2) . . . . ?
C1 C6 C5 C4 0.6(3) . . . . ?
C1 C2 C3 C4 0.8(3) . . . . ?
C6 C1 C2 C3 0.3(3) . . . . ?
C6 C5 C4 C3 0.5(3) . . . . ?
C2 C1 C6 C7 179.46(17) . . . . ?
C2 C1 C6 C5 -1.0(3) . . . . ?
C2 C3 C4 C5 -1.1(3) . . . . ?
C7 C6 C5 C4 -179.82(18) . . . . ?
C5 C6 C7 C8 -63.1(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 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.652
####################################################################### 
# 
# 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_C18H22O2Os
_database_code_depnum_ccdc_archive 'CCDC 2119165'
loop_
_audit_author_name
_audit_author_address
'Thomas Saal'
;University of Southern California
United States of America
;
_audit_update_record             
;
2021-10-29 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_chemical_name_systematic        Dimesityldioxoosmium(VI)
_chemical_name_common            OsO2(mes)2
_chemical_formula_moiety         'C18 H22 O2 Os'
_chemical_formula_sum            'C18 H22 O2 Os'
_chemical_formula_iupac          ?
_chemical_formula_weight         460.55

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.6400(4)
_cell_length_b                   15.1376(5)
_cell_length_c                   8.2955(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.2720(10)
_cell_angle_gamma                90
_cell_volume                     1570.74(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8686
_cell_measurement_theta_min      4.5857
_cell_measurement_theta_max      71.9238
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.066
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888

_exptl_absorpt_coefficient_mu    15.341
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_absorpt_correction_T_min  0.15
_exptl_absorpt_correction_T_max  0.43

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'luS microsource'
_diffrn_source_type              ?

_diffrn_radiation_type           'CuK\a '
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            22437
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_theta_min         3.53
_diffrn_reflns_theta_max         71.92
_diffrn_reflns_theta_full        71.92
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_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       -10
_diffrn_reflns_limit_l_max       10

_refine_special_details          
;
;

_reflns_number_total             3056
_reflns_number_gt                2876
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0584
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_number_reflns         3056
_refine_ls_number_parameters     196
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0288P)²+1.5592P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.825
_refine_diff_density_min         -1.406
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -4.9801 6.2216 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2018.1-0 (Bruker AXS, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2017)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XT 2017/1 (Bruker AXS, 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 882)'
_computing_publication_material  'SHELXTL XT 2017/1 (Bruker AXS, 2017)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os1 0.75229(2) 0.48114(2) 0.56615(2) 0.01415(7) Uani d . . . 1 . .
O O1 0.75803(19) 0.58181(15) 0.6592(3) 0.0211(5) Uani d . . . 1 . .
O O2 0.75831(19) 0.44275(17) 0.3747(3) 0.0233(5) Uani d . . . 1 . .
C C1 0.8652(3) 0.4031(2) 0.7004(4) 0.0134(6) Uani d . . . 1 . .
C C2 0.8502(3) 0.3121(2) 0.7314(4) 0.0151(7) Uani d . . . 1 . .
C C3 0.9291(3) 0.2682(2) 0.8359(4) 0.0167(7) Uani d . . . 1 . .
H H3 0.919006 0.207483 0.858661 0.02 Uiso calc U . R 1 . .
C C4 1.0222(3) 0.3096(2) 0.9081(4) 0.0168(7) Uani d . . . 1 . .
C C5 1.0381(3) 0.3974(2) 0.8671(4) 0.0171(7) Uani d . . . 1 . .
H H5 1.102665 0.425905 0.911738 0.021 Uiso calc U . R 1 . .
C C6 0.9626(3) 0.4446(2) 0.7631(4) 0.0147(7) Uani d . . . 1 . .
C C7 0.7560(3) 0.2583(2) 0.6514(5) 0.0205(7) Uani d . . . 1 . .
H H7A 0.737523 0.276679 0.53756 0.031 Uiso calc U . R 1 . .
H H7B 0.694616 0.267979 0.709202 0.031 Uiso calc U . R 1 . .
H H7C 0.77496 0.195512 0.655732 0.031 Uiso calc U . R 1 . .
C C8 1.1059(3) 0.2587(2) 1.0187(5) 0.0219(8) Uani d . . . 1 . .
H H8A 1.153094 0.228124 0.953106 0.033 Uiso calc U . R 1 . .
H H8B 1.070879 0.2153 1.081029 0.033 Uiso calc U . R 1 . .
H H8C 1.147995 0.299627 1.093879 0.033 Uiso calc U . R 1 . .
C C9 0.9894(3) 0.5390(2) 0.7229(4) 0.0180(7) Uani d . . . 1 . .
H H9A 0.972566 0.54843 0.605143 0.027 Uiso calc U . R 1 . .
H H9B 1.065671 0.549758 0.757848 0.027 Uiso calc U . R 1 . .
H H9C 0.947173 0.57973 0.779822 0.027 Uiso calc U . R 1 . .
C C10 0.6231(3) 0.42595(19) 0.6540(4) 0.0142(6) Uani d . . . 1 . .
C C11 0.6166(3) 0.4267(2) 0.8235(4) 0.0153(7) Uani d . . . 1 . .
C C12 0.5247(3) 0.3942(2) 0.8773(4) 0.0163(7) Uani d . . . 1 . .
H H12 0.51991 0.395838 0.99053 0.02 Uiso calc U . R 1 . .
C C13 0.4394(3) 0.3595(2) 0.7709(4) 0.0167(7) Uani d . . . 1 . .
C C14 0.4481(3) 0.3590(2) 0.6056(4) 0.0167(7) Uani d . . . 1 . .
H H14 0.391099 0.334868 0.531486 0.02 Uiso calc U . R 1 . .
C C15 0.5372(3) 0.39238(19) 0.5445(4) 0.0150(7) Uani d . . . 1 . .
C C16 0.7012(3) 0.4659(2) 0.9492(4) 0.0190(7) Uani d . . . 1 . .
H H16A 0.769674 0.436552 0.943766 0.029 Uiso calc U . R 1 . .
H H16B 0.680932 0.457519 1.057904 0.029 Uiso calc U . R 1 . .
H H16C 0.708027 0.529181 0.928024 0.029 Uiso calc U . R 1 . .
C C17 0.3399(3) 0.3260(2) 0.8302(5) 0.0220(7) Uani d . . . 1 . .
H H17A 0.28009 0.365638 0.7929 0.033 Uiso calc U . R 1 . .
H H17B 0.351281 0.323912 0.949559 0.033 Uiso calc U . R 1 . .
H H17C 0.323444 0.266535 0.786956 0.033 Uiso calc U . R 1 . .
C C18 0.5357(3) 0.3881(2) 0.3623(4) 0.0179(7) Uani d . . . 1 . .
H H18A 0.466229 0.365795 0.310674 0.027 Uiso calc U . R 1 . .
H H18B 0.592407 0.348319 0.337447 0.027 Uiso calc U . R 1 . .
H H18C 0.547593 0.447266 0.320599 0.027 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Os1 O2 . 1.703(3) ?
Os1 O1 . 1.705(2) ?
Os1 C1 . 2.053(3) ?
Os1 C10 . 2.059(3) ?
C1 C6 . 1.412(5) ?
C1 C2 . 1.419(4) ?
C2 C3 . 1.393(5) ?
C2 C7 . 1.514(4) ?
C3 C4 . 1.391(5) ?
C3 H3 . 0.95 ?
C4 C5 . 1.393(5) ?
C4 C8 . 1.509(5) ?
C5 C6 . 1.389(5) ?
C5 H5 . 0.95 ?
C6 C9 . 1.517(4) ?
C7 H7A . 0.98 ?
C7 H7B . 0.98 ?
C7 H7C . 0.98 ?
C8 H8A . 0.98 ?
C8 H8B . 0.98 ?
C8 H8C . 0.98 ?
C9 H9A . 0.98 ?
C9 H9B . 0.98 ?
C9 H9C . 0.98 ?
C10 C15 . 1.407(5) ?
C10 C11 . 1.420(5) ?
C11 C12 . 1.393(5) ?
C11 C16 . 1.504(5) ?
C12 C13 . 1.394(5) ?
C12 H12 . 0.95 ?
C13 C14 . 1.391(5) ?
C13 C17 . 1.504(5) ?
C14 C15 . 1.395(5) ?
C14 H14 . 0.95 ?
C15 C18 . 1.510(5) ?
C16 H16A . 0.98 ?
C16 H16B . 0.98 ?
C16 H16C . 0.98 ?
C17 H17A . 0.98 ?
C17 H17B . 0.98 ?
C17 H17C . 0.98 ?
C18 H18A . 0.98 ?
C18 H18B . 0.98 ?
C18 H18C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Os1 O1 . . 136.26(12) ?
O2 Os1 C1 . . 100.88(12) ?
O1 Os1 C1 . . 106.70(12) ?
O2 Os1 C10 . . 109.63(12) ?
O1 Os1 C10 . . 100.75(12) ?
C1 Os1 C10 . . 95.72(12) ?
C6 C1 C2 . . 119.8(3) ?
C6 C1 Os1 . . 116.4(2) ?
C2 C1 Os1 . . 123.7(2) ?
C3 C2 C1 . . 118.3(3) ?
C3 C2 C7 . . 117.6(3) ?
C1 C2 C7 . . 124.1(3) ?
C4 C3 C2 . . 122.5(3) ?
C4 C3 H3 . . 118.7 ?
C2 C3 H3 . . 118.7 ?
C3 C4 C5 . . 117.9(3) ?
C3 C4 C8 . . 120.4(3) ?
C5 C4 C8 . . 121.5(3) ?
C6 C5 C4 . . 122.1(3) ?
C6 C5 H5 . . 119.0 ?
C4 C5 H5 . . 119.0 ?
C5 C6 C1 . . 119.0(3) ?
C5 C6 C9 . . 117.7(3) ?
C1 C6 C9 . . 123.2(3) ?
C2 C7 H7A . . 109.5 ?
C2 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C2 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C4 C8 H8A . . 109.5 ?
C4 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C4 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C6 C9 H9A . . 109.5 ?
C6 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C6 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C15 C10 C11 . . 119.6(3) ?
C15 C10 Os1 . . 119.7(2) ?
C11 C10 Os1 . . 120.6(2) ?
C12 C11 C10 . . 118.9(3) ?
C12 C11 C16 . . 117.3(3) ?
C10 C11 C16 . . 123.6(3) ?
C11 C12 C13 . . 122.3(3) ?
C11 C12 H12 . . 118.9 ?
C13 C12 H12 . . 118.9 ?
C14 C13 C12 . . 117.6(3) ?
C14 C13 C17 . . 120.6(3) ?
C12 C13 C17 . . 121.8(3) ?
C13 C14 C15 . . 122.6(3) ?
C13 C14 H14 . . 118.7 ?
C15 C14 H14 . . 118.7 ?
C14 C15 C10 . . 119.0(3) ?
C14 C15 C18 . . 117.0(3) ?
C10 C15 C18 . . 124.0(3) ?
C11 C16 H16A . . 109.5 ?
C11 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C11 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C13 C17 H17A . . 109.5 ?
C13 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C13 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C15 C18 H18A . . 109.5 ?
C15 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C15 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . 5.7(5) ?
Os1 C1 C2 C3 . . . . -174.6(2) ?
C6 C1 C2 C7 . . . . -171.1(3) ?
Os1 C1 C2 C7 . . . . 8.6(5) ?
C1 C2 C3 C4 . . . . -1.1(5) ?
C7 C2 C3 C4 . . . . 176.0(3) ?
C2 C3 C4 C5 . . . . -3.1(5) ?
C2 C3 C4 C8 . . . . -179.2(3) ?
C3 C4 C5 C6 . . . . 2.7(5) ?
C8 C4 C5 C6 . . . . 178.8(3) ?
C4 C5 C6 C1 . . . . 1.9(5) ?
C4 C5 C6 C9 . . . . -178.3(3) ?
C2 C1 C6 C5 . . . . -6.1(5) ?
Os1 C1 C6 C5 . . . . 174.1(2) ?
C2 C1 C6 C9 . . . . 174.1(3) ?
Os1 C1 C6 C9 . . . . -5.6(4) ?
C15 C10 C11 C12 . . . . -0.2(4) ?
Os1 C10 C11 C12 . . . . 175.6(2) ?
C15 C10 C11 C16 . . . . -176.3(3) ?
Os1 C10 C11 C16 . . . . -0.5(4) ?
C10 C11 C12 C13 . . . . 1.2(5) ?
C16 C11 C12 C13 . . . . 177.6(3) ?
C11 C12 C13 C14 . . . . -0.7(5) ?
C11 C12 C13 C17 . . . . -179.0(3) ?
C12 C13 C14 C15 . . . . -0.8(5) ?
C17 C13 C14 C15 . . . . 177.6(3) ?
C13 C14 C15 C10 . . . . 1.7(5) ?
C13 C14 C15 C18 . . . . -179.7(3) ?
C11 C10 C15 C14 . . . . -1.2(4) ?
Os1 C10 C15 C14 . . . . -177.1(2) ?
C11 C10 C15 C18 . . . . -179.7(3) ?
Os1 C10 C15 C18 . . . . 4.4(4) ?



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

data_C36H44Os
_database_code_depnum_ccdc_archive 'CCDC 2175534'
loop_
_audit_author_name
_audit_author_address
'Thomas Saal'
;University of Southern California
United States of America
;
_audit_update_record             
;
2022-05-28 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_chemical_name_systematic        tetrakis(2-isopropylphenyl)osmium(IV)
_chemical_name_common            Os1-iPr
_chemical_formula_moiety         'C36 H44 Os'
_chemical_formula_sum            'C36 H44 Os'
_chemical_formula_iupac          ?
_chemical_formula_weight         666.91
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'P -4'
_space_group_name_Hall           'P -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'

_cell_length_a                   11.904(4)
_cell_length_b                   11.904(4)
_cell_length_c                   10.580(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1499.2(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9993
_cell_measurement_theta_min      2.4195
_cell_measurement_theta_max      30.3242
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark purple'
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.033
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672

_exptl_absorpt_coefficient_mu    4.274
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_T_max  0.87

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            37981
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15

_refine_special_details          
;

Refined as a 2-component inversion twin.
;

_reflns_number_total             4494
_reflns_number_gt                3983
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0205
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0420
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_number_reflns         4494
_refine_ls_number_parameters     173
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²+0.2196P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.963
_refine_diff_density_min         -1.103
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.231(9)

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'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX2 v2018.1-0 (Bruker AXS, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 882)'
_computing_publication_material  'SHELXTL XT 2017/1 (Bruker AXS, 2017)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.6314(3) 0.0323(3) 0.2432(3) 0.0131(7) Uani d . . . 1 . .
C C2 0.6252(3) 0.1204(3) 0.1541(4) 0.0166(7) Uani d . . . 1 . .
C C3 0.7193(3) 0.1418(3) 0.0784(4) 0.0222(8) Uani d . . . 1 . .
H H3 0.716332 0.20048 0.017625 0.027 Uiso calc U . R 1 . .
C C4 0.8176(3) 0.0784(3) 0.0907(4) 0.0230(8) Uani d . . . 1 . .
H H4 0.880929 0.095522 0.039624 0.028 Uiso calc U . R 1 . .
C C5 0.8233(5) -0.0083(5) 0.1757(6) 0.0209(12) Uani d . . . 1 . .
H H5 0.890077 -0.051485 0.183425 0.025 Uiso calc U . R 1 . .
C C6 0.7290(3) -0.0329(3) 0.2518(4) 0.0170(8) Uani d . . . 1 . .
H H6 0.731731 -0.094176 0.309212 0.02 Uiso calc U . R 1 . .
C C7 0.5171(3) 0.1873(3) 0.1354(4) 0.0186(7) Uani d . . . 1 . .
H H7 0.46436 0.164523 0.204343 0.022 Uiso calc U . R 1 . .
C C8 0.5343(5) 0.3133(4) 0.1471(7) 0.0253(13) Uani d . . . 1 . .
H H8A 0.586214 0.338865 0.081241 0.038 Uiso calc U . R 1 . .
H H8B 0.565791 0.330664 0.230457 0.038 Uiso calc U . R 1 . .
H H8C 0.462009 0.351703 0.137276 0.038 Uiso calc U . R 1 . .
C C9 0.4024(3) 0.1353(3) 0.5756(4) 0.0152(7) Uani d . . . 1 . .
C C10 0.4601(4) 0.1579(4) 0.0097(4) 0.0260(9) Uani d . . . 1 . .
H H10A 0.511119 0.175167 -0.060315 0.039 Uiso calc U . R 1 . .
H H10B 0.391061 0.202003 0.00067 0.039 Uiso calc U . R 1 . .
H H10C 0.441664 0.077653 0.008486 0.039 Uiso calc U . R 1 . .
C C11 0.4836(3) 0.1302(3) 0.4780(3) 0.0128(7) Uani d . . . 1 . .
C C12 0.4124(3) 0.2189(3) 0.6668(4) 0.0178(8) Uani d . . . 1 . .
H H12 0.358714 0.222625 0.733122 0.021 Uiso calc U . R 1 . .
C C13 0.4997(3) 0.2978(3) 0.6635(4) 0.0196(8) Uani d . . . 1 . .
H H13 0.505179 0.353375 0.727605 0.024 Uiso calc U . R 1 . .
C C14 0.5777(4) 0.2947(5) 0.5670(7) 0.0193(12) Uani d . . . 1 . .
H H14 0.636481 0.348645 0.563754 0.023 Uiso calc U . R 1 . .
C C15 0.5696(3) 0.2119(3) 0.4744(4) 0.0163(7) Uani d . . . 1 . .
H H15 0.622834 0.210379 0.407499 0.02 Uiso calc U . R 1 . .
C C16 0.3069(3) 0.0496(3) 0.5864(4) 0.0166(7) Uani d . . . 1 . .
H H16 0.312918 -0.002505 0.512562 0.02 Uiso calc U . R 1 . .
C C17 0.3174(4) -0.0210(4) 0.7066(4) 0.0223(8) Uani d . . . 1 . .
H H17A 0.260819 -0.08078 0.705458 0.033 Uiso calc U . R 1 . .
H H17B 0.305473 0.02697 0.780668 0.033 Uiso calc U . R 1 . .
H H17C 0.392548 -0.054351 0.710611 0.033 Uiso calc U . R 1 . .
C C18 0.1920(5) 0.1072(4) 0.5791(7) 0.0211(12) Uani d . . . 1 . .
H H18A 0.18851 0.15395 0.502933 0.032 Uiso calc U . R 1 . .
H H18B 0.181227 0.154468 0.653967 0.032 Uiso calc U . R 1 . .
H H18C 0.132827 0.050095 0.575725 0.032 Uiso calc U . R 1 . .
Os Os01 0.5 0 0.35787(2) 0.01237(5) Uani d T P S 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C6 . 1.400(5) ?
C1 C2 . 1.412(5) ?
C1 Os01 . 2.016(3) ?
C2 C3 . 1.401(6) ?
C2 C7 . 1.527(5) ?
C3 C4 . 1.398(6) ?
C3 H3 . 0.95 ?
C4 C5 . 1.371(8) ?
C4 H4 . 0.95 ?
C5 C6 . 1.412(7) ?
C5 H5 . 0.95 ?
C6 H6 . 0.95 ?
C7 C8 . 1.519(6) ?
C7 C10 . 1.533(6) ?
C7 H7 . 1.0 ?
C8 H8A . 0.98 ?
C8 H8B . 0.98 ?
C8 H8C . 0.98 ?
C9 C12 . 1.393(5) ?
C9 C11 . 1.416(5) ?
C9 C16 . 1.531(5) ?
C10 H10A . 0.98 ?
C10 H10B . 0.98 ?
C10 H10C . 0.98 ?
C11 C15 . 1.413(5) ?
C11 Os01 . 2.014(4) ?
C12 C13 . 1.400(5) ?
C12 H12 . 0.95 ?
C13 C14 . 1.381(8) ?
C13 H13 . 0.95 ?
C14 C15 . 1.393(7) ?
C14 H14 . 0.95 ?
C15 H15 . 0.95 ?
C16 C17 . 1.530(6) ?
C16 C18 . 1.532(6) ?
C16 H16 . 1.0 ?
C17 H17A . 0.98 ?
C17 H17B . 0.98 ?
C17 H17C . 0.98 ?
C18 H18A . 0.98 ?
C18 H18B . 0.98 ?
C18 H18C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 C1 C2 . . 119.9(3) ?
C6 C1 Os01 . . 119.9(3) ?
C2 C1 Os01 . . 120.2(3) ?
C3 C2 C1 . . 118.4(3) ?
C3 C2 C7 . . 120.3(4) ?
C1 C2 C7 . . 121.2(3) ?
C4 C3 C2 . . 121.2(4) ?
C4 C3 H3 . . 119.4 ?
C2 C3 H3 . . 119.4 ?
C5 C4 C3 . . 120.6(4) ?
C5 C4 H4 . . 119.7 ?
C3 C4 H4 . . 119.7 ?
C4 C5 C6 . . 119.4(5) ?
C4 C5 H5 . . 120.3 ?
C6 C5 H5 . . 120.3 ?
C1 C6 C5 . . 120.6(4) ?
C1 C6 H6 . . 119.7 ?
C5 C6 H6 . . 119.7 ?
C8 C7 C2 . . 113.0(4) ?
C8 C7 C10 . . 110.9(4) ?
C2 C7 C10 . . 111.5(3) ?
C8 C7 H7 . . 107.0 ?
C2 C7 H7 . . 107.0 ?
C10 C7 H7 . . 107.0 ?
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 ?
C12 C9 C11 . . 118.5(3) ?
C12 C9 C16 . . 119.2(4) ?
C11 C9 C16 . . 122.2(3) ?
C7 C10 H10A . . 109.5 ?
C7 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C7 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C15 C11 C9 . . 119.0(3) ?
C15 C11 Os01 . . 116.3(3) ?
C9 C11 Os01 . . 124.0(3) ?
C9 C12 C13 . . 121.7(4) ?
C9 C12 H12 . . 119.1 ?
C13 C12 H12 . . 119.1 ?
C14 C13 C12 . . 120.0(4) ?
C14 C13 H13 . . 120.0 ?
C12 C13 H13 . . 120.0 ?
C13 C14 C15 . . 119.5(4) ?
C13 C14 H14 . . 120.3 ?
C15 C14 H14 . . 120.3 ?
C14 C15 C11 . . 121.2(4) ?
C14 C15 H15 . . 119.4 ?
C11 C15 H15 . . 119.4 ?
C17 C16 C9 . . 111.6(3) ?
C17 C16 C18 . . 111.1(4) ?
C9 C16 C18 . . 111.2(3) ?
C17 C16 H16 . . 107.6 ?
C9 C16 H16 . . 107.6 ?
C18 C16 H16 . . 107.6 ?
C16 C17 H17A . . 109.5 ?
C16 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C16 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C16 C18 H18A . . 109.5 ?
C16 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C16 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C11 Os01 C11 2_655 . 101.7(2) ?
C11 Os01 C1 2_655 2_655 107.95(14) ?
C11 Os01 C1 . 2_655 116.84(14) ?
C11 Os01 C1 2_655 . 116.84(14) ?
C11 Os01 C1 . . 107.95(14) ?
C1 Os01 C1 2_655 . 106.0(2) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . -1.7(6) ?
Os01 C1 C2 C3 . . . . 178.5(3) ?
C6 C1 C2 C7 . . . . 175.3(4) ?
Os01 C1 C2 C7 . . . . -4.5(5) ?
C1 C2 C3 C4 . . . . -0.4(6) ?
C7 C2 C3 C4 . . . . -177.4(4) ?
C2 C3 C4 C5 . . . . 1.4(7) ?
C3 C4 C5 C6 . . . . -0.4(7) ?
C2 C1 C6 C5 . . . . 2.7(6) ?
Os01 C1 C6 C5 . . . . -177.4(3) ?
C4 C5 C6 C1 . . . . -1.7(7) ?
C3 C2 C7 C8 . . . . -56.5(6) ?
C1 C2 C7 C8 . . . . 126.6(5) ?
C3 C2 C7 C10 . . . . 69.2(5) ?
C1 C2 C7 C10 . . . . -107.7(4) ?
C12 C9 C11 C15 . . . . -2.1(5) ?
C16 C9 C11 C15 . . . . -179.8(3) ?
C12 C9 C11 Os01 . . . . 168.1(3) ?
C16 C9 C11 Os01 . . . . -9.6(5) ?
C11 C9 C12 C13 . . . . 0.6(6) ?
C16 C9 C12 C13 . . . . 178.4(4) ?
C9 C12 C13 C14 . . . . 0.9(7) ?
C12 C13 C14 C15 . . . . -0.8(8) ?
C13 C14 C15 C11 . . . . -0.7(7) ?
C9 C11 C15 C14 . . . . 2.1(6) ?
Os01 C11 C15 C14 . . . . -168.8(4) ?
C12 C9 C16 C17 . . . . -62.8(5) ?
C11 C9 C16 C17 . . . . 114.8(4) ?
C12 C9 C16 C18 . . . . 61.8(6) ?
C11 C9 C16 C18 . . . . -120.5(5) ?



####################################################################### 
# 
# 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_C36H44Os_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2024176'
loop_
_audit_author_name
_audit_author_address
'Ralf Haiges'
;University of Southern California
United States of America
;
_audit_update_record             
;
2020-08-19 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_chemical_name_systematic        tetrakis(2,4,6-trimethylphenyl)osmium(IV)
_chemical_name_common            Os(mesityl)4
_chemical_formula_moiety         'C36 H44 Os'
_chemical_formula_sum            'C36 H44 Os'
_chemical_formula_iupac          ?
_chemical_formula_weight         666.91

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_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                   16.265(3)
_cell_length_b                   24.149(5)
_cell_length_c                   14.951(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.736(3)
_cell_angle_gamma                90
_cell_volume                     5860.(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9858
_cell_measurement_theta_min      2.7305
_cell_measurement_theta_max      30.4915
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       rod
_exptl_crystal_colour            'dark black'
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.051
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2688

_exptl_absorpt_coefficient_mu    4.374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_absorpt_correction_T_min  0.11
_exptl_absorpt_correction_T_max  0.80

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'fine-focus tube'
_diffrn_source_type              ?

_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'

_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            59569
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19

_refine_special_details          
;

Refined as a 2-component twin.
;

_reflns_number_total             6726
_reflns_number_gt                5752
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0676
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_restrained_S_all      1.160
_refine_ls_number_reflns         6726
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0244P)²+29.8209P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.992
_refine_diff_density_min         -1.230
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2018/3 (Bruker AXS, 2018)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 958)'
_computing_publication_material  'SHELXTL XL 2018/3 (Bruker AXS, 2018)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.8225(2) 0.59408(14) 0.5897(2) 0.0174(6) Uani d . . . 1 . .
C C2 0.8637(2) 0.55144(14) 0.5452(2) 0.0191(7) Uani d . . . 1 . .
C C3 0.8497(2) 0.48994(15) 0.5569(3) 0.0269(8) Uani d . . . 1 . .
H H3A 0.792131 0.483395 0.569534 0.04 Uiso calc U . R 1 . .
H H3B 0.885984 0.476152 0.60684 0.04 Uiso calc U . R 1 . .
H H3C 0.861873 0.470473 0.50175 0.04 Uiso calc U . R 1 . .
C C4 0.9217(2) 0.56544(15) 0.4836(2) 0.0187(6) Uani d . . . 1 . .
H H4 0.951018 0.53652 0.456763 0.022 Uiso calc U . R 1 . .
C C5 0.9380(2) 0.61983(15) 0.4603(2) 0.0198(7) Uani d . . . 1 . .
C C6 0.9971(2) 0.63298(17) 0.3890(3) 0.0272(8) Uani d . . . 1 . .
H H6A 0.975292 0.618131 0.331197 0.041 Uiso calc U . R 1 . .
H H6B 1.050794 0.6161 0.405311 0.041 Uiso calc U . R 1 . .
H H6C 1.003497 0.673206 0.384252 0.041 Uiso calc U . R 1 . .
C C7 0.8963(2) 0.66148(15) 0.5025(2) 0.0204(7) Uani d . . . 1 . .
H H7 0.906345 0.699003 0.487611 0.024 Uiso calc U . R 1 . .
C C8 0.8399(2) 0.64963(14) 0.5664(2) 0.0198(7) Uani d . . . 1 . .
C C9 0.7985(2) 0.69860(15) 0.6079(3) 0.0269(8) Uani d . . . 1 . .
H H9A 0.836069 0.730381 0.610058 0.04 Uiso calc U . R 1 . .
H H9B 0.784642 0.689085 0.668793 0.04 Uiso calc U . R 1 . .
H H9C 0.748108 0.708044 0.571618 0.04 Uiso calc U . R 1 . .
C C10 0.7145(2) 0.50300(14) 0.7114(2) 0.0175(6) Uani d . . . 1 . .
C C11 0.6412(2) 0.47180(14) 0.6960(2) 0.0177(6) Uani d . . . 1 . .
C C12 0.5636(2) 0.49282(14) 0.6462(2) 0.0208(7) Uani d . . . 1 . .
H H12A 0.559937 0.477927 0.585095 0.031 Uiso calc U . R 1 . .
H H12B 0.564896 0.533364 0.643847 0.031 Uiso calc U . R 1 . .
H H12C 0.515483 0.480798 0.677373 0.031 Uiso calc U . R 1 . .
C C13 0.6384(2) 0.41713(14) 0.7278(2) 0.0195(7) Uani d . . . 1 . .
H H13 0.58843 0.396985 0.718538 0.023 Uiso calc U . R 1 . .
C C14 0.7053(2) 0.39134(14) 0.7721(2) 0.0220(7) Uani d . . . 1 . .
C C15 0.7010(3) 0.33249(15) 0.8053(3) 0.0286(8) Uani d . . . 1 . .
H H15A 0.646789 0.31684 0.787344 0.043 Uiso calc U . R 1 . .
H H15B 0.709343 0.332017 0.870801 0.043 Uiso calc U . R 1 . .
H H15C 0.743952 0.310381 0.779317 0.043 Uiso calc U . R 1 . .
C C16 0.7773(2) 0.42182(14) 0.7862(2) 0.0202(7) Uani d . . . 1 . .
H H16 0.82409 0.404782 0.815872 0.024 Uiso calc U . R 1 . .
C C17 0.7830(2) 0.47652(14) 0.7582(2) 0.0190(7) Uani d . . . 1 . .
C C18 0.8636(2) 0.50671(16) 0.7787(3) 0.0248(7) Uani d . . . 1 . .
H H18A 0.909115 0.480058 0.780991 0.037 Uiso calc U . R 1 . .
H H18B 0.86227 0.525495 0.836704 0.037 Uiso calc U . R 1 . .
H H18C 0.871556 0.534109 0.731713 0.037 Uiso calc U . R 1 . .
C C19 0.6390(2) 0.62274(14) 0.6079(2) 0.0178(6) Uani d . . . 1 . .
C C20 0.5985(2) 0.67156(14) 0.6340(2) 0.0195(7) Uani d . . . 1 . .
C C21 0.6137(2) 0.70108(15) 0.7231(3) 0.0251(8) Uani d . . . 1 . .
H H21A 0.601945 0.740645 0.71523 0.038 Uiso calc U . R 1 . .
H H21B 0.671371 0.696155 0.744913 0.038 Uiso calc U . R 1 . .
H H21C 0.577646 0.685509 0.766713 0.038 Uiso calc U . R 1 . .
C C22 0.5402(2) 0.69624(14) 0.5735(3) 0.0224(7) Uani d . . . 1 . .
H H22 0.512515 0.728465 0.59218 0.027 Uiso calc U . R 1 . .
C C23 0.5208(2) 0.67618(15) 0.4880(3) 0.0236(7) Uani d . . . 1 . .
C C24 0.4619(3) 0.70649(17) 0.4229(3) 0.0350(10) Uani d . . . 1 . .
H H24A 0.491693 0.7356 0.392659 0.052 Uiso calc U . R 1 . .
H H24B 0.417811 0.723191 0.455411 0.052 Uiso calc U . R 1 . .
H H24C 0.438114 0.680361 0.378202 0.052 Uiso calc U . R 1 . .
C C25 0.5604(2) 0.62794(14) 0.4630(2) 0.0221(7) Uani d . . . 1 . .
H H25 0.547675 0.612819 0.405105 0.027 Uiso calc U . R 1 . .
C C26 0.6183(2) 0.60133(14) 0.5212(2) 0.0185(7) Uani d . . . 1 . .
C C27 0.6591(2) 0.54990(15) 0.4862(2) 0.0217(7) Uani d . . . 1 . .
H H27A 0.618292 0.527969 0.450558 0.032 Uiso calc U . R 1 . .
H H27B 0.681897 0.527705 0.536854 0.032 Uiso calc U . R 1 . .
H H27C 0.703631 0.560802 0.448714 0.032 Uiso calc U . R 1 . .
C C28 0.7559(2) 0.61446(14) 0.8038(2) 0.0180(6) Uani d . . . 1 . .
C C29 0.6905(2) 0.60931(14) 0.8627(2) 0.0177(6) Uani d . . . 1 . .
C C30 0.6098(2) 0.58143(14) 0.8334(2) 0.0192(7) Uani d . . . 1 . .
H H30A 0.597272 0.587873 0.769282 0.029 Uiso calc U . R 1 . .
H H30B 0.565549 0.596841 0.867338 0.029 Uiso calc U . R 1 . .
H H30C 0.614301 0.541541 0.844753 0.029 Uiso calc U . R 1 . .
C C31 0.6990(2) 0.63008(15) 0.9494(2) 0.0206(7) Uani d . . . 1 . .
H H31 0.654477 0.626097 0.986958 0.025 Uiso calc U . R 1 . .
C C32 0.7704(2) 0.65651(15) 0.9834(2) 0.0216(7) Uani d . . . 1 . .
C C33 0.7783(2) 0.68028(18) 1.0769(3) 0.0302(8) Uani d . . . 1 . .
H H33A 0.824954 0.705997 1.082087 0.045 Uiso calc U . R 1 . .
H H33B 0.787438 0.65021 1.12041 0.045 Uiso calc U . R 1 . .
H H33C 0.727562 0.700077 1.088873 0.045 Uiso calc U . R 1 . .
C C34 0.8349(2) 0.65993(15) 0.9268(2) 0.0223(7) Uani d . . . 1 . .
H H34 0.884933 0.676736 0.948978 0.027 Uiso calc U . R 1 . .
C C35 0.8294(2) 0.63980(15) 0.8388(2) 0.0209(7) Uani d . . . 1 . .
C C36 0.9064(2) 0.64629(18) 0.7885(3) 0.0300(9) Uani d . . . 1 . .
H H36A 0.89908 0.627229 0.730647 0.045 Uiso calc U . R 1 . .
H H36B 0.953399 0.630132 0.823705 0.045 Uiso calc U . R 1 . .
H H36C 0.916795 0.685708 0.778443 0.045 Uiso calc U . R 1 . .
Os Os1 0.73302(2) 0.58319(2) 0.67841(2) 0.01409(5) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.418(5) ?
C1 C8 . 1.419(5) ?
C1 Os1 . 2.049(3) ?
C2 C4 . 1.401(5) ?
C2 C3 . 1.514(5) ?
C3 H3A . 0.98 ?
C3 H3B . 0.98 ?
C3 H3C . 0.98 ?
C4 C5 . 1.389(5) ?
C4 H4 . 0.95 ?
C5 C7 . 1.388(5) ?
C5 C6 . 1.515(5) ?
C6 H6A . 0.98 ?
C6 H6B . 0.98 ?
C6 H6C . 0.98 ?
C7 C8 . 1.396(5) ?
C7 H7 . 0.95 ?
C8 C9 . 1.513(5) ?
C9 H9A . 0.98 ?
C9 H9B . 0.98 ?
C9 H9C . 0.98 ?
C10 C11 . 1.417(5) ?
C10 C17 . 1.427(5) ?
C10 Os1 . 2.026(3) ?
C11 C13 . 1.405(5) ?
C11 C12 . 1.511(5) ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 C14 . 1.383(5) ?
C13 H13 . 0.95 ?
C14 C16 . 1.387(5) ?
C14 C15 . 1.508(5) ?
C15 H15A . 0.98 ?
C15 H15B . 0.98 ?
C15 H15C . 0.98 ?
C16 C17 . 1.391(5) ?
C16 H16 . 0.95 ?
C17 C18 . 1.514(5) ?
C18 H18A . 0.98 ?
C18 H18B . 0.98 ?
C18 H18C . 0.98 ?
C19 C26 . 1.416(5) ?
C19 C20 . 1.418(5) ?
C19 Os1 . 2.037(3) ?
C20 C22 . 1.399(5) ?
C20 C21 . 1.517(5) ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C22 C23 . 1.385(5) ?
C22 H22 . 0.95 ?
C23 C25 . 1.394(5) ?
C23 C24 . 1.510(5) ?
C24 H24A . 0.98 ?
C24 H24B . 0.98 ?
C24 H24C . 0.98 ?
C25 C26 . 1.397(5) ?
C25 H25 . 0.95 ?
C26 C27 . 1.517(5) ?
C27 H27A . 0.98 ?
C27 H27B . 0.98 ?
C27 H27C . 0.98 ?
C28 C35 . 1.413(5) ?
C28 C29 . 1.430(4) ?
C28 Os1 . 2.033(3) ?
C29 C31 . 1.388(5) ?
C29 C30 . 1.514(5) ?
C30 H30A . 0.98 ?
C30 H30B . 0.98 ?
C30 H30C . 0.98 ?
C31 C32 . 1.391(5) ?
C31 H31 . 0.95 ?
C32 C34 . 1.392(5) ?
C32 C33 . 1.509(5) ?
C33 H33A . 0.98 ?
C33 H33B . 0.98 ?
C33 H33C . 0.98 ?
C34 C35 . 1.400(5) ?
C34 H34 . 0.95 ?
C35 C36 . 1.511(5) ?
C36 H36A . 0.98 ?
C36 H36B . 0.98 ?
C36 H36C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C8 . . 117.6(3) ?
C2 C1 Os1 . . 126.0(2) ?
C8 C1 Os1 . . 116.2(2) ?
C4 C2 C1 . . 119.5(3) ?
C4 C2 C3 . . 115.2(3) ?
C1 C2 C3 . . 125.4(3) ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C5 C4 C2 . . 122.8(3) ?
C5 C4 H4 . . 118.6 ?
C2 C4 H4 . . 118.6 ?
C7 C5 C4 . . 117.6(3) ?
C7 C5 C6 . . 121.3(3) ?
C4 C5 C6 . . 121.1(3) ?
C5 C6 H6A . . 109.5 ?
C5 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C5 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
C5 C7 C8 . . 121.7(3) ?
C5 C7 H7 . . 119.2 ?
C8 C7 H7 . . 119.2 ?
C7 C8 C1 . . 120.8(3) ?
C7 C8 C9 . . 116.7(3) ?
C1 C8 C9 . . 122.5(3) ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C8 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C11 C10 C17 . . 117.6(3) ?
C11 C10 Os1 . . 127.3(2) ?
C17 C10 Os1 . . 115.1(2) ?
C13 C11 C10 . . 119.3(3) ?
C13 C11 C12 . . 116.0(3) ?
C10 C11 C12 . . 124.7(3) ?
C11 C12 H12A . . 109.5 ?
C11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C14 C13 C11 . . 122.9(3) ?
C14 C13 H13 . . 118.5 ?
C11 C13 H13 . . 118.5 ?
C13 C14 C16 . . 117.6(3) ?
C13 C14 C15 . . 122.0(3) ?
C16 C14 C15 . . 120.4(3) ?
C14 C15 H15A . . 109.5 ?
C14 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C14 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
C14 C16 C17 . . 122.1(3) ?
C14 C16 H16 . . 119.0 ?
C17 C16 H16 . . 119.0 ?
C16 C17 C10 . . 120.5(3) ?
C16 C17 C18 . . 118.1(3) ?
C10 C17 C18 . . 121.4(3) ?
C17 C18 H18A . . 109.5 ?
C17 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C17 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C26 C19 C20 . . 117.9(3) ?
C26 C19 Os1 . . 115.4(2) ?
C20 C19 Os1 . . 126.5(3) ?
C22 C20 C19 . . 119.0(3) ?
C22 C20 C21 . . 115.6(3) ?
C19 C20 C21 . . 125.4(3) ?
C20 C21 H21A . . 109.5 ?
C20 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C20 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C23 C22 C20 . . 123.5(3) ?
C23 C22 H22 . . 118.3 ?
C20 C22 H22 . . 118.3 ?
C22 C23 C25 . . 117.3(3) ?
C22 C23 C24 . . 121.5(3) ?
C25 C23 C24 . . 121.1(4) ?
C23 C24 H24A . . 109.5 ?
C23 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C23 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
C23 C25 C26 . . 121.5(3) ?
C23 C25 H25 . . 119.3 ?
C26 C25 H25 . . 119.3 ?
C25 C26 C19 . . 120.9(3) ?
C25 C26 C27 . . 117.1(3) ?
C19 C26 C27 . . 122.1(3) ?
C26 C27 H27A . . 109.5 ?
C26 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
C26 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
C35 C28 C29 . . 117.1(3) ?
C35 C28 Os1 . . 127.0(2) ?
C29 C28 Os1 . . 115.9(2) ?
C31 C29 C28 . . 120.7(3) ?
C31 C29 C30 . . 117.6(3) ?
C28 C29 C30 . . 121.8(3) ?
C29 C30 H30A . . 109.5 ?
C29 C30 H30B . . 109.5 ?
H30A C30 H30B . . 109.5 ?
C29 C30 H30C . . 109.5 ?
H30A C30 H30C . . 109.5 ?
H30B C30 H30C . . 109.5 ?
C29 C31 C32 . . 122.5(3) ?
C29 C31 H31 . . 118.7 ?
C32 C31 H31 . . 118.7 ?
C31 C32 C34 . . 116.7(3) ?
C31 C32 C33 . . 122.1(3) ?
C34 C32 C33 . . 121.2(3) ?
C32 C33 H33A . . 109.5 ?
C32 C33 H33B . . 109.5 ?
H33A C33 H33B . . 109.5 ?
C32 C33 H33C . . 109.5 ?
H33A C33 H33C . . 109.5 ?
H33B C33 H33C . . 109.5 ?
C32 C34 C35 . . 123.1(3) ?
C32 C34 H34 . . 118.4 ?
C35 C34 H34 . . 118.4 ?
C34 C35 C28 . . 119.9(3) ?
C34 C35 C36 . . 115.4(3) ?
C28 C35 C36 . . 124.7(3) ?
C35 C36 H36A . . 109.5 ?
C35 C36 H36B . . 109.5 ?
H36A C36 H36B . . 109.5 ?
C35 C36 H36C . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
C10 Os1 C28 . . 98.71(13) ?
C10 Os1 C19 . . 117.12(13) ?
C28 Os1 C19 . . 112.90(14) ?
C10 Os1 C1 . . 113.79(13) ?
C28 Os1 C1 . . 117.04(13) ?
C19 Os1 C1 . . 98.37(13) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C8 C1 C2 C4 . . . . 2.6(5) ?
Os1 C1 C2 C4 . . . . 177.7(2) ?
C8 C1 C2 C3 . . . . -176.2(3) ?
Os1 C1 C2 C3 . . . . -1.1(5) ?
C1 C2 C4 C5 . . . . -3.4(5) ?
C3 C2 C4 C5 . . . . 175.5(3) ?
C2 C4 C5 C7 . . . . 2.0(5) ?
C2 C4 C5 C6 . . . . -176.0(3) ?
C4 C5 C7 C8 . . . . 0.1(5) ?
C6 C5 C7 C8 . . . . 178.1(3) ?
C5 C7 C8 C1 . . . . -0.7(5) ?
C5 C7 C8 C9 . . . . 179.8(3) ?
C2 C1 C8 C7 . . . . -0.6(5) ?
Os1 C1 C8 C7 . . . . -176.2(3) ?
C2 C1 C8 C9 . . . . 178.8(3) ?
Os1 C1 C8 C9 . . . . 3.2(4) ?
C17 C10 C11 C13 . . . . 0.8(5) ?
Os1 C10 C11 C13 . . . . -176.7(2) ?
C17 C10 C11 C12 . . . . -178.8(3) ?
Os1 C10 C11 C12 . . . . 3.7(5) ?
C10 C11 C13 C14 . . . . -1.8(5) ?
C12 C11 C13 C14 . . . . 177.9(3) ?
C11 C13 C14 C16 . . . . 1.0(5) ?
C11 C13 C14 C15 . . . . -179.7(3) ?
C13 C14 C16 C17 . . . . 0.7(5) ?
C15 C14 C16 C17 . . . . -178.6(3) ?
C14 C16 C17 C10 . . . . -1.6(5) ?
C14 C16 C17 C18 . . . . 178.5(3) ?
C11 C10 C17 C16 . . . . 0.8(5) ?
Os1 C10 C17 C16 . . . . 178.6(3) ?
C11 C10 C17 C18 . . . . -179.3(3) ?
Os1 C10 C17 C18 . . . . -1.5(4) ?
C26 C19 C20 C22 . . . . 0.0(5) ?
Os1 C19 C20 C22 . . . . 174.0(2) ?
C26 C19 C20 C21 . . . . -178.7(3) ?
Os1 C19 C20 C21 . . . . -4.8(5) ?
C19 C20 C22 C23 . . . . -1.4(5) ?
C21 C20 C22 C23 . . . . 177.5(3) ?
C20 C22 C23 C25 . . . . 1.9(5) ?
C20 C22 C23 C24 . . . . -175.6(3) ?
C22 C23 C25 C26 . . . . -1.1(5) ?
C24 C23 C25 C26 . . . . 176.4(3) ?
C23 C25 C26 C19 . . . . -0.2(5) ?
C23 C25 C26 C27 . . . . -178.5(3) ?
C20 C19 C26 C25 . . . . 0.7(5) ?
Os1 C19 C26 C25 . . . . -173.9(3) ?
C20 C19 C26 C27 . . . . 179.0(3) ?
Os1 C19 C26 C27 . . . . 4.4(4) ?
C35 C28 C29 C31 . . . . 1.9(5) ?
Os1 C28 C29 C31 . . . . -178.9(3) ?
C35 C28 C29 C30 . . . . -178.2(3) ?
Os1 C28 C29 C30 . . . . 0.9(4) ?
C28 C29 C31 C32 . . . . -0.1(5) ?
C30 C29 C31 C32 . . . . -179.9(3) ?
C29 C31 C32 C34 . . . . -1.8(5) ?
C29 C31 C32 C33 . . . . 178.3(4) ?
C31 C32 C34 C35 . . . . 1.9(5) ?
C33 C32 C34 C35 . . . . -178.2(4) ?
C32 C34 C35 C28 . . . . -0.1(6) ?
C32 C34 C35 C36 . . . . -178.8(4) ?
C29 C28 C35 C34 . . . . -1.8(5) ?
Os1 C28 C35 C34 . . . . 179.2(3) ?
C29 C28 C35 C36 . . . . 176.8(3) ?
Os1 C28 C35 C36 . . . . -2.3(5) ?



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
