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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_jy105
_database_code_depnum_ccdc_archive 'CCDC 1859533'
_audit_update_record             
;
2018-08-01 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
Chlorido-(1-methyl-4-isopropyl-benzene)-(N-n-butyl-(phenyl)(methylester)benzimidazol-\kN,C)osmium(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H33 Cl N2 O2 Os'
_chemical_formula_sum            'C29 H33 Cl N2 O2 Os'
_chemical_formula_weight         667.22

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

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

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

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

_cell_length_a                   11.0472(6)
_cell_length_b                   19.7668(10)
_cell_length_c                   12.2934(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.1612(18)
_cell_angle_gamma                90
_cell_volume                     2468.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9768
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      30.49

_exptl_crystal_description       prisms
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_F_000             1320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.076
_exptl_absorpt_coefficient_mu    5.305
_shelx_estimated_absorpt_T_min   0.633
_shelx_estimated_absorpt_T_max   0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6476
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 QUEST CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            103770
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.061
_diffrn_reflns_theta_max         30.598
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7582
_reflns_number_gt                6178
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2017)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

Hydrogen atoms for aromatic CH, aliphatic CH, CH₂ and methyl
groups were positioned geometrically (C---H = 0.95 Å for aromatic CH, C---H
= 1.00 Å for aliphatic CH, C---H = 0.99 Å for CH₂, C---H = 0.98 Å for
CH₃) and refined using a riding model (AFIX 43 for aromatic CH, 
AFIX 13 for CH, AFIX 23 for CH₂, AFIX 137 for rotating group for CH₃), 
with Uiso(H) = 1.2Ueq(CH,CH₂) and Uiso(H) = 1.5Ueq(CH₃).

The largest residual electron density peaks of 2.45 and 2.16 e Å⁻³ are
within  1.0 Å from
the Os atom, the deepest hole of -1.76 e Å⁻³ is 0.77 Å from the C5 atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+15.4911P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7582
_refine_ls_number_parameters     321
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.0632
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.06300(2) 0.21956(2) 0.84296(2) 0.00990(4) Uani 1 1 d . . . . .
Cl Cl -0.00637(9) 0.12136(5) 0.71638(8) 0.01456(18) Uani 1 1 d . . . . .
O1 O 0.5658(3) 0.06199(14) 1.0868(3) 0.0172(6) Uani 1 1 d . . . . .
O2 O 0.5660(3) -0.02374(15) 1.2082(3) 0.0174(6) Uani 1 1 d . . . . .
N1 N 0.0785(3) 0.14901(16) 0.9748(3) 0.0108(6) Uani 1 1 d . . . . .
N2 N -0.0094(3) 0.08400(16) 1.0739(3) 0.0102(6) Uani 1 1 d . . . . .
C1 C 0.1902(4) 0.2507(2) 0.7421(4) 0.0167(8) Uani 1 1 d . . . . .
C2 C 0.0726(4) 0.2896(2) 0.7088(3) 0.0164(8) Uani 1 1 d . . . . .
H2 H 0.0139 0.2918 0.6280 0.020 Uiso 1 1 calc R U . . .
C3 C 0.0423(4) 0.32504(19) 0.7954(4) 0.0155(8) Uani 1 1 d . . . . .
H3 H -0.0358 0.3514 0.7707 0.019 Uiso 1 1 calc R U . . .
C4 C 0.1253(4) 0.32237(19) 0.9179(3) 0.0149(8) Uani 1 1 d . . . . .
C5 C 0.2370(3) 0.2793(2) 0.9491(3) 0.0131(7) Uani 1 1 d . . . . .
H5 H 0.2897 0.2723 1.0306 0.016 Uiso 1 1 calc R U . . .
C6 C 0.2732(4) 0.2460(2) 0.8628(4) 0.0160(8) Uani 1 1 d . . . . .
H6 H 0.3426 0.2101 0.8892 0.019 Uiso 1 1 calc R U . . .
C7 C 0.2190(4) 0.2131(2) 0.6488(4) 0.0224(9) Uani 1 1 d . . . . .
H7A H 0.1502 0.1793 0.6118 0.034 Uiso 1 1 calc R U . . .
H7B H 0.3046 0.1905 0.6852 0.034 Uiso 1 1 calc R U . . .
H7C H 0.2212 0.2451 0.5887 0.034 Uiso 1 1 calc R U . . .
C8 C 0.1027(4) 0.3670(2) 1.0084(4) 0.0196(9) Uani 1 1 d . . . . .
H8 H 0.1585 0.3491 1.0886 0.024 Uiso 1 1 calc R U . . .
C9 C -0.0398(5) 0.3687(2) 0.9982(4) 0.0270(10) Uani 1 1 d . . . . .
H9A H -0.0958 0.3896 0.9229 0.041 Uiso 1 1 calc R U . . .
H9B H -0.0448 0.3952 1.0637 0.041 Uiso 1 1 calc R U . . .
H9C H -0.0702 0.3225 1.0015 0.041 Uiso 1 1 calc R U . . .
C10 C 0.1525(4) 0.4382(2) 0.9981(4) 0.0216(9) Uani 1 1 d . . . . .
H10A H 0.1015 0.4564 0.9191 0.032 Uiso 1 1 calc R U . . .
H10B H 0.2457 0.4359 1.0107 0.032 Uiso 1 1 calc R U . . .
H10C H 0.1422 0.4677 1.0579 0.032 Uiso 1 1 calc R U . . .
C11 C -0.0301(4) 0.13548(19) 0.9941(3) 0.0107(7) Uani 1 1 d . . . . .
C12 C 0.1192(4) 0.06226(19) 1.1047(3) 0.0110(7) Uani 1 1 d . . . . .
C13 C 0.1898(4) 0.00994(19) 1.1786(3) 0.0127(7) Uani 1 1 d . . . . .
H13 H 0.1527 -0.0171 1.2214 0.015 Uiso 1 1 calc R U . . .
C14 C 0.3166(4) -0.0005(2) 1.1862(3) 0.0136(8) Uani 1 1 d . . . . .
H14 H 0.3675 -0.0358 1.2353 0.016 Uiso 1 1 calc R U . . .
C15 C 0.3725(4) 0.03954(19) 1.1237(3) 0.0108(7) Uani 1 1 d . . . . .
C16 C 0.3019(4) 0.09230(18) 1.0504(3) 0.0098(7) Uani 1 1 d . . . . .
H16 H 0.3396 0.1197 1.0084 0.012 Uiso 1 1 calc R U . . .
C17 C 0.1739(4) 0.10299(18) 1.0417(3) 0.0104(7) Uani 1 1 d . . . . .
C18 C -0.0965(4) 0.0610(2) 1.1311(3) 0.0134(8) Uani 1 1 d . . . . .
H18A H -0.0629 0.0178 1.1729 0.016 Uiso 1 1 calc R U . . .
H18B H -0.1857 0.0527 1.0700 0.016 Uiso 1 1 calc R U . . .
C19 C -0.1044(4) 0.1139(2) 1.2197(4) 0.0173(8) Uani 1 1 d . . . . .
H19A H -0.1237 0.1585 1.1801 0.021 Uiso 1 1 calc R U . . .
H19B H -0.1790 0.1021 1.2417 0.021 Uiso 1 1 calc R U . . .
C20 C 0.0196(5) 0.1199(2) 1.3321(4) 0.0235(9) Uani 1 1 d . . . . .
H20A H 0.0970 0.1222 1.3105 0.028 Uiso 1 1 calc R U . . .
H20B H 0.0162 0.1627 1.3725 0.028 Uiso 1 1 calc R U . . .
C21 C 0.0377(5) 0.0616(3) 1.4170(4) 0.0326(11) Uani 1 1 d . . . . .
H21A H 0.0333 0.0187 1.3756 0.049 Uiso 1 1 calc R U . . .
H21B H -0.0321 0.0628 1.4473 0.049 Uiso 1 1 calc R U . . .
H21C H 0.1237 0.0655 1.4831 0.049 Uiso 1 1 calc R U . . .
C22 C 0.5106(4) 0.02817(19) 1.1350(3) 0.0122(7) Uani 1 1 d . . . . .
C23 C 0.7019(4) -0.0378(2) 1.2310(4) 0.0233(9) Uani 1 1 d . . . . .
H23A H 0.7138 -0.0381 1.1561 0.035 Uiso 1 1 calc R U . . .
H23B H 0.7263 -0.0820 1.2694 0.035 Uiso 1 1 calc R U . . .
H23C H 0.7580 -0.0027 1.2830 0.035 Uiso 1 1 calc R U . . .
C24 C -0.1486(4) 0.17188(19) 0.9220(3) 0.0120(7) Uani 1 1 d . . . . .
C25 C -0.2754(4) 0.1624(2) 0.9214(3) 0.0157(8) Uani 1 1 d . . . . .
H25 H -0.2880 0.1334 0.9777 0.019 Uiso 1 1 calc R U . . .
C26 C -0.3810(4) 0.1958(2) 0.8380(4) 0.0210(9) Uani 1 1 d . . . . .
H26 H -0.4671 0.1891 0.8357 0.025 Uiso 1 1 calc R U . . .
C27 C -0.3616(4) 0.2391(2) 0.7575(4) 0.0188(9) Uani 1 1 d . . . . .
H27 H -0.4347 0.2618 0.7002 0.023 Uiso 1 1 calc R U . . .
C28 C -0.2362(4) 0.2496(2) 0.7601(4) 0.0156(8) Uani 1 1 d . . . . .
H28 H -0.2252 0.2802 0.7052 0.019 Uiso 1 1 calc R U . . .
C29 C -0.1250(3) 0.2162(2) 0.8416(3) 0.0118(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os C29 2.071(4) . ?
Os N1 2.093(3) . ?
Os C3 2.153(4) . ?
Os C2 2.187(4) . ?
Os C5 2.195(4) . ?
Os C4 2.226(4) . ?
Os C1 2.294(4) . ?
Os C6 2.298(4) . ?
Os Cl 2.4164(9) . ?
O1 C22 1.206(5) . ?
O2 C22 1.343(5) . ?
O2 C23 1.442(5) . ?
N1 C11 1.339(5) . ?
N1 C17 1.390(5) . ?
N2 C11 1.368(5) . ?
N2 C12 1.387(5) . ?
N2 C18 1.470(5) . ?
C1 C6 1.408(6) . ?
C1 C2 1.424(6) . ?
C1 C7 1.501(6) . ?
C2 C3 1.419(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.423(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.422(5) . ?
C4 C8 1.515(6) . ?
C5 C6 1.433(6) . ?
C5 H5 0.9500 . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.530(6) . ?
C8 C10 1.535(6) . ?
C8 H8 1.0000 . ?
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 C24 1.451(5) . ?
C12 C13 1.394(5) . ?
C12 C17 1.408(5) . ?
C13 C14 1.382(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.404(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.398(5) . ?
C15 C22 1.493(5) . ?
C16 C17 1.391(5) . ?
C16 H16 0.9500 . ?
C18 C19 1.537(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.521(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.515(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.410(5) . ?
C24 C29 1.420(5) . ?
C25 C26 1.381(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.389(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.407(5) . ?
C28 H28 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
C29 Os N1 76.22(14) . . ?
C29 Os C3 91.70(16) . . ?
N1 Os C3 145.40(14) . . ?
C29 Os C2 111.08(15) . . ?
N1 Os C2 172.64(14) . . ?
C3 Os C2 38.16(15) . . ?
C29 Os C5 131.50(14) . . ?
N1 Os C5 96.44(13) . . ?
C3 Os C5 67.37(15) . . ?
C2 Os C5 79.46(14) . . ?
C29 Os C4 100.28(15) . . ?
N1 Os C4 111.74(13) . . ?
C3 Os C4 37.88(15) . . ?
C2 Os C4 68.60(15) . . ?
C5 Os C4 37.51(15) . . ?
C29 Os C1 146.05(15) . . ?
N1 Os C1 135.74(14) . . ?
C3 Os C1 67.38(16) . . ?
C2 Os C1 36.96(15) . . ?
C5 Os C1 66.29(14) . . ?
C4 Os C1 79.81(15) . . ?
C29 Os C6 167.52(15) . . ?
N1 Os C6 107.31(13) . . ?
C3 Os C6 78.67(15) . . ?
C2 Os C6 65.77(15) . . ?
C5 Os C6 37.11(14) . . ?
C4 Os C6 67.24(15) . . ?
C1 Os C6 35.71(14) . . ?
C29 Os Cl 84.62(11) . . ?
N1 Os Cl 82.64(9) . . ?
C3 Os Cl 129.05(11) . . ?
C2 Os Cl 96.89(11) . . ?
C5 Os Cl 142.81(11) . . ?
C4 Os Cl 165.49(10) . . ?
C1 Os Cl 88.50(11) . . ?
C6 Os Cl 107.59(11) . . ?
C22 O2 C23 116.3(3) . . ?
C11 N1 C17 106.7(3) . . ?
C11 N1 Os 117.7(2) . . ?
C17 N1 Os 135.0(3) . . ?
C11 N2 C12 106.9(3) . . ?
C11 N2 C18 128.1(3) . . ?
C12 N2 C18 124.5(3) . . ?
C6 C1 C2 118.7(4) . . ?
C6 C1 C7 121.7(4) . . ?
C2 C1 C7 119.4(4) . . ?
C6 C1 Os 72.3(2) . . ?
C2 C1 Os 67.5(2) . . ?
C7 C1 Os 129.7(3) . . ?
C3 C2 C1 120.6(4) . . ?
C3 C2 Os 69.6(2) . . ?
C1 C2 Os 75.6(2) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
Os C2 H2 127.0 . . ?
C2 C3 C4 122.1(4) . . ?
C2 C3 Os 72.2(2) . . ?
C4 C3 Os 73.8(2) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
Os C3 H3 127.1 . . ?
C5 C4 C3 116.0(4) . . ?
C5 C4 C8 121.7(4) . . ?
C3 C4 C8 122.1(4) . . ?
C5 C4 Os 70.1(2) . . ?
C3 C4 Os 68.3(2) . . ?
C8 C4 Os 136.2(3) . . ?
C4 C5 C6 122.7(3) . . ?
C4 C5 Os 72.4(2) . . ?
C6 C5 Os 75.3(2) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
Os C5 H5 125.4 . . ?
C1 C6 C5 119.6(4) . . ?
C1 C6 Os 72.0(2) . . ?
C5 C6 Os 67.5(2) . . ?
C1 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
Os C6 H6 119.2 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 C9 114.5(4) . . ?
C4 C8 C10 107.8(3) . . ?
C9 C8 C10 111.3(4) . . ?
C4 C8 H8 107.7 . . ?
C9 C8 H8 107.7 . . ?
C10 C8 H8 107.7 . . ?
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 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 N2 111.5(3) . . ?
N1 C11 C24 116.6(3) . . ?
N2 C11 C24 131.5(3) . . ?
N2 C12 C13 131.2(3) . . ?
N2 C12 C17 106.7(3) . . ?
C13 C12 C17 122.1(3) . . ?
C14 C13 C12 116.5(3) . . ?
C14 C13 H13 121.7 . . ?
C12 C13 H13 121.7 . . ?
C13 C14 C15 122.1(4) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C16 C15 C14 121.2(3) . . ?
C16 C15 C22 117.6(3) . . ?
C14 C15 C22 121.2(3) . . ?
C17 C16 C15 117.1(3) . . ?
C17 C16 H16 121.4 . . ?
C15 C16 H16 121.4 . . ?
N1 C17 C16 131.0(3) . . ?
N1 C17 C12 108.1(3) . . ?
C16 C17 C12 120.9(3) . . ?
N2 C18 C19 111.0(3) . . ?
N2 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
N2 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 114.5(3) . . ?
C20 C19 H19A 108.6 . . ?
C18 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C21 C20 C19 113.2(4) . . ?
C21 C20 H20A 108.9 . . ?
C19 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.8 . . ?
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 . . ?
O1 C22 O2 124.6(4) . . ?
O1 C22 C15 124.5(4) . . ?
O2 C22 C15 110.9(3) . . ?
O2 C23 H23A 109.5 . . ?
O2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 122.2(3) . . ?
C25 C24 C11 126.4(4) . . ?
C29 C24 C11 111.3(3) . . ?
C26 C25 C24 119.2(4) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C25 C26 C27 120.1(4) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C28 120.5(4) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C28 C29 122.1(4) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 H28 119.0 . . ?
C28 C29 C24 115.9(3) . . ?
C28 C29 Os 125.7(3) . . ?
C24 C29 Os 118.2(3) . . ?

_refine_diff_density_max         2.451
_refine_diff_density_min         -1.757
_refine_diff_density_rms         0.201


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methylene chloride, hexane, toluene'
####################################################################### 
# 
# 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_jY85
_database_code_depnum_ccdc_archive 'CCDC 1859534'
_audit_update_record             
;
2018-08-01 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'Acetato-(1-methyl-4-isopropyl-benzene)-(N-n-butyl-(4-biphenyl)(methylester)benzimidazol-\kN,C)osmium(II)hemi-dichloromethane, hemi-toluene solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H40 N2 O4 Os, 0.5(C7 H8), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C41 H45 Cl N2 O4 Os'
_chemical_formula_weight         855.44

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9559(6)
_cell_length_b                   10.9932(6)
_cell_length_c                   16.2594(9)
_cell_angle_alpha                105.966(2)
_cell_angle_beta                 102.536(2)
_cell_angle_gamma                103.578(2)
_cell_volume                     1745.05(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9621
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      28.37

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_F_000             860
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.126
_exptl_absorpt_coefficient_mu    3.776
_shelx_estimated_absorpt_T_min   0.500
_shelx_estimated_absorpt_T_max   0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6233
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 QUEST CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            85900
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.005
_diffrn_reflns_theta_max         28.389
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8746
_reflns_number_gt                7910
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2017)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

Hydrogen atoms for aromatic CH, aliphatic CH, CH₂ and methyl
groups were positioned geometrically (C---H = 0.95 Å for aromatic CH, C---H
= 1.00 Å for aliphatic CH, C---H = 0.99 Å for CH₂, C---H = 0.98 Å for
CH₃) and refined using a riding model (AFIX 43 for aromatic CH, 
AFIX 13 for CH, AFIX 23 for CH₂, AFIX 137 for rotating group for CH₃), 
with Uiso(H) = 1.2Ueq(CH,CH₂) and Uiso(H) = 1.5Ueq(CH₃).

The dichloromethane and toluene crystal solvent molecules share a common
position. They were both refined to half-occupancy with PART commands. For
toluene the PART -n command was used as the toluene molecule sits 
around the inversion center.
The phenyl ring of the toluene molecule was refined as a rigid group 
using AFIX 66 1.39 to fits the following next six non-H atoms to a 
regular hexagon with C-C = 1.39 Å.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0112P)²+3.9323P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8746
_refine_ls_number_parameters     482
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0530
_refine_ls_wR_factor_gt          0.0511
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.12021(2) 1.02450(2) 0.27458(2) 0.01486(4) Uani 1 1 d . . . . .
O1 O -0.2086(2) 0.3498(2) -0.05366(14) 0.0330(5) Uani 1 1 d . . . . .
O2 O -0.1679(2) 0.5603(2) -0.05095(13) 0.0295(5) Uani 1 1 d . . . . .
O3 O -0.0711(2) 1.0321(2) 0.26813(13) 0.0206(4) Uani 1 1 d . . . . .
O4 O -0.0274(2) 1.2520(2) 0.33910(15) 0.0275(5) Uani 1 1 d . . . . .
N5 N 0.0415(2) 0.8389(2) 0.28461(14) 0.0143(4) Uani 1 1 d . . . . .
N8 N 0.0142(2) 0.7007(2) 0.36188(15) 0.0140(4) Uani 1 1 d . . . . .
C1 C 0.1157(3) 1.1218(3) 0.16988(19) 0.0229(6) Uani 1 1 d . . . . .
C2 C 0.2132(3) 1.2074(3) 0.25287(19) 0.0211(6) Uani 1 1 d . . . . .
H2 H 0.2130 1.2959 0.2794 0.025 Uiso 1 1 calc R U . . .
C3 C 0.3096(3) 1.1603(3) 0.29546(19) 0.0203(6) Uani 1 1 d . . . . .
H3 H 0.3733 1.2187 0.3505 0.024 Uiso 1 1 calc R U . . .
C4 C 0.3153(3) 1.0284(3) 0.25893(19) 0.0206(6) Uani 1 1 d . . . . .
C5 C 0.2150(3) 0.9452(3) 0.17783(19) 0.0204(6) Uani 1 1 d . . . . .
H5 H 0.2108 0.8546 0.1538 0.025 Uiso 1 1 calc R U . . .
C6 C 0.1203(3) 0.9913(3) 0.13079(19) 0.0230(6) Uani 1 1 d . . . . .
H6 H 0.0607 0.9349 0.0737 0.028 Uiso 1 1 calc R U . . .
C7 C 0.0073(3) 1.1668(3) 0.1279(2) 0.0283(7) Uani 1 1 d . . . . .
H7A H 0.0317 1.2036 0.0832 0.042 Uiso 1 1 calc R U . . .
H7B H -0.0073 1.2354 0.1743 0.042 Uiso 1 1 calc R U . . .
H7C H -0.0736 1.0908 0.0987 0.042 Uiso 1 1 calc R U . . .
C8 C 0.4202(3) 0.9779(3) 0.3030(2) 0.0257(7) Uani 1 1 d . . . . .
H8 H 0.4824 0.9732 0.2662 0.031 Uiso 1 1 calc R U . . .
C9 C 0.3640(4) 0.8373(3) 0.3045(3) 0.0393(9) Uani 1 1 d . . . . .
H9A H 0.4364 0.8054 0.3270 0.059 Uiso 1 1 calc R U . . .
H9B H 0.3119 0.7772 0.2437 0.059 Uiso 1 1 calc R U . . .
H9C H 0.3078 0.8394 0.3439 0.059 Uiso 1 1 calc R U . . .
C10 C 0.5009(3) 1.0693(3) 0.3977(2) 0.0328(7) Uani 1 1 d . . . . .
H10A H 0.5667 1.0313 0.4222 0.049 Uiso 1 1 calc R U . . .
H10B H 0.4426 1.0786 0.4355 0.049 Uiso 1 1 calc R U . . .
H10C H 0.5455 1.1570 0.3967 0.049 Uiso 1 1 calc R U . . .
C11 C 0.0606(3) 0.8304(3) 0.36666(17) 0.0135(5) Uani 1 1 d . . . . .
C12 C -0.0381(3) 0.6236(3) 0.27221(17) 0.0149(5) Uani 1 1 d . . . . .
C13 C -0.0964(3) 0.4860(3) 0.22911(19) 0.0185(6) Uani 1 1 d . . . . .
H13 H -0.1065 0.4271 0.2621 0.022 Uiso 1 1 calc R U . . .
C14 C -0.1387(3) 0.4396(3) 0.13634(19) 0.0203(6) Uani 1 1 d . . . . .
H14 H -0.1795 0.3468 0.1048 0.024 Uiso 1 1 calc R U . . .
C15 C -0.1227(3) 0.5270(3) 0.08757(19) 0.0201(6) Uani 1 1 d . . . . .
C16 C -0.0635(3) 0.6636(3) 0.13061(18) 0.0182(6) Uani 1 1 d . . . . .
H16 H -0.0524 0.7224 0.0976 0.022 Uiso 1 1 calc R U . . .
C17 C -0.0214(3) 0.7108(3) 0.22378(17) 0.0151(5) Uani 1 1 d . . . . .
C18 C 0.0355(3) 0.6465(3) 0.43526(18) 0.0162(5) Uani 1 1 d . . . . .
H18A H -0.0216 0.5528 0.4140 0.019 Uiso 1 1 calc R U . . .
H18B H 0.0108 0.6981 0.4857 0.019 Uiso 1 1 calc R U . . .
C19 C 0.1791(3) 0.6528(3) 0.46802(18) 0.0180(6) Uani 1 1 d . . . . .
H19A H 0.1929 0.6283 0.5227 0.022 Uiso 1 1 calc R U . . .
H19B H 0.2361 0.7456 0.4844 0.022 Uiso 1 1 calc R U . . .
C20 C 0.2208(3) 0.5606(3) 0.3980(2) 0.0231(6) Uani 1 1 d . . . . .
H20A H 0.1705 0.4670 0.3866 0.028 Uiso 1 1 calc R U . . .
H20B H 0.1976 0.5784 0.3411 0.028 Uiso 1 1 calc R U . . .
C21 C 0.3678(3) 0.5774(3) 0.4263(2) 0.0269(7) Uani 1 1 d . . . . .
H21A H 0.3885 0.5172 0.3783 0.040 Uiso 1 1 calc R U . . .
H21B H 0.3909 0.5560 0.4811 0.040 Uiso 1 1 calc R U . . .
H21C H 0.4184 0.6697 0.4375 0.040 Uiso 1 1 calc R U . . .
C22 C -0.1702(3) 0.4677(3) -0.01177(19) 0.0223(6) Uani 1 1 d . . . . .
C23 C -0.2143(4) 0.5090(3) -0.1479(2) 0.0315(7) Uani 1 1 d . . . . .
H23A H -0.2202 0.5822 -0.1704 0.047 Uiso 1 1 calc R U . . .
H23B H -0.3015 0.4423 -0.1682 0.047 Uiso 1 1 calc R U . . .
H23C H -0.1527 0.4679 -0.1709 0.047 Uiso 1 1 calc R U . . .
C24 C 0.1247(3) 0.9546(3) 0.44114(17) 0.0143(5) Uani 1 1 d . . . . .
C25 C 0.1456(3) 0.9722(3) 0.53240(18) 0.0164(5) Uani 1 1 d . . . . .
H25 H 0.1193 0.8976 0.5505 0.020 Uiso 1 1 calc R U . . .
C26 C 0.2047(3) 1.0984(3) 0.59592(18) 0.0164(5) Uani 1 1 d . . . . .
H26 H 0.2185 1.1099 0.6577 0.020 Uiso 1 1 calc R U . . .
C27 C 0.2444(3) 1.2095(3) 0.57046(18) 0.0154(5) Uani 1 1 d . . . . .
C28 C 0.2196(3) 1.1900(3) 0.47879(18) 0.0162(5) Uani 1 1 d . . . . .
H28 H 0.2445 1.2655 0.4612 0.019 Uiso 1 1 calc R U . . .
C29 C 0.1597(3) 1.0641(3) 0.41180(17) 0.0146(5) Uani 1 1 d . . . . .
C30 C 0.3103(3) 1.3454(3) 0.63913(18) 0.0176(6) Uani 1 1 d . . . . .
C31 C 0.3768(3) 1.3634(3) 0.7275(2) 0.0254(7) Uani 1 1 d . . . . .
H31 H 0.3791 1.2878 0.7445 0.030 Uiso 1 1 calc R U . . .
C32 C 0.4395(3) 1.4904(3) 0.7908(2) 0.0322(8) Uani 1 1 d . . . . .
H32 H 0.4830 1.5005 0.8507 0.039 Uiso 1 1 calc R U . . .
C33 C 0.4392(3) 1.6017(3) 0.7675(2) 0.0312(7) Uani 1 1 d . . . . .
H33 H 0.4834 1.6883 0.8107 0.037 Uiso 1 1 calc R U . . .
C34 C 0.3741(3) 1.5860(3) 0.6806(2) 0.0272(7) Uani 1 1 d . . . . .
H34 H 0.3736 1.6623 0.6640 0.033 Uiso 1 1 calc R U . . .
C35 C 0.3091(3) 1.4590(3) 0.6172(2) 0.0210(6) Uani 1 1 d . . . . .
H35 H 0.2631 1.4498 0.5580 0.025 Uiso 1 1 calc R U . . .
C36 C -0.1030(3) 1.1391(3) 0.29428(19) 0.0213(6) Uani 1 1 d . . . . .
C37 C -0.2496(3) 1.1150(3) 0.2634(2) 0.0319(7) Uani 1 1 d . . . . .
H37A H -0.2686 1.1679 0.2255 0.048 Uiso 1 1 calc R U . . .
H37B H -0.2808 1.1411 0.3157 0.048 Uiso 1 1 calc R U . . .
H37C H -0.2946 1.0202 0.2290 0.048 Uiso 1 1 calc R U . . .
C38 C 0.6844(9) 0.7638(12) 0.0832(7) 0.059(3) Uani 0.5 1 d . . P A 1
H38A H 0.7396 0.8332 0.1414 0.071 Uiso 0.5 1 calc R U P A 1
H38B H 0.7064 0.6808 0.0808 0.071 Uiso 0.5 1 calc R U P A 1
Cl1 Cl 0.7220(2) 0.8141(3) -0.00369(16) 0.0606(6) Uani 0.5 1 d . . P A 1
Cl2 Cl 0.5168(2) 0.7357(3) 0.0777(2) 0.0705(7) Uani 0.5 1 d . . P A 1
C39 C 0.4188(9) 0.1846(8) -0.0298(6) 0.112(6) Uani 0.5 1 d G . P B -2
C40 C 0.5215(9) 0.1488(9) -0.0564(6) 0.085(4) Uani 0.5 1 d G . P B -2
H40 H 0.5767 0.2049 -0.0779 0.102 Uiso 0.5 1 calc R U P B -2
C41 C 0.5434(9) 0.0311(11) -0.0516(8) 0.183(12) Uani 0.5 1 d G . P B -2
H41 H 0.6136 0.0067 -0.0697 0.219 Uiso 0.5 1 calc R U P B -2
C42 C 0.4625(10) -0.0509(10) -0.0202(8) 0.150(9) Uani 0.5 1 d G . P B -2
H42 H 0.4775 -0.1314 -0.0169 0.180 Uiso 0.5 1 calc R U P B -2
C43 C 0.3598(8) -0.0152(9) 0.0064(7) 0.115(6) Uani 0.5 1 d G . P B -2
H43 H 0.3046 -0.0712 0.0278 0.138 Uiso 0.5 1 calc R U P B -2
C44 C 0.3379(7) 0.1026(9) 0.0015(5) 0.078(3) Uani 0.5 1 d G . P B -2
H44 H 0.2677 0.1270 0.0197 0.093 Uiso 0.5 1 calc R U P B -2
C45 C 0.408(2) 0.3195(19) -0.0445(9) 0.145(9) Uani 0.5 1 d . . P B -2
H45A H 0.3611 0.3005 -0.1074 0.217 Uiso 0.5 1 calc R U P B -2
H45B H 0.4969 0.3816 -0.0290 0.217 Uiso 0.5 1 calc R U P B -2
H45C H 0.3603 0.3594 -0.0060 0.217 Uiso 0.5 1 calc R U P B -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os C29 2.077(3) . ?
Os N5 2.086(2) . ?
Os O3 2.099(2) . ?
Os C3 2.148(3) . ?
Os C5 2.167(3) . ?
Os C2 2.188(3) . ?
Os C4 2.198(3) . ?
Os C1 2.243(3) . ?
Os C6 2.265(3) . ?
O1 C22 1.206(4) . ?
O2 C22 1.340(4) . ?
O2 C23 1.446(3) . ?
O3 C36 1.292(3) . ?
O4 C36 1.231(4) . ?
N5 C11 1.338(3) . ?
N5 C17 1.385(3) . ?
N8 C11 1.371(3) . ?
N8 C12 1.379(3) . ?
N8 C18 1.473(3) . ?
C1 C6 1.418(4) . ?
C1 C2 1.432(4) . ?
C1 C7 1.494(4) . ?
C2 C3 1.414(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.430(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.421(4) . ?
C4 C8 1.518(4) . ?
C5 C6 1.426(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.517(4) . ?
C8 C9 1.533(5) . ?
C8 H8 1.0000 . ?
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 C24 1.447(4) . ?
C12 C13 1.398(4) . ?
C12 C17 1.403(4) . ?
C13 C14 1.383(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.408(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.391(4) . ?
C15 C22 1.484(4) . ?
C16 C17 1.389(4) . ?
C16 H16 0.9500 . ?
C18 C19 1.526(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.530(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.527(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.402(4) . ?
C24 C29 1.415(4) . ?
C25 C26 1.382(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.400(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.401(4) . ?
C27 C30 1.492(4) . ?
C28 C29 1.402(4) . ?
C28 H28 0.9500 . ?
C30 C35 1.393(4) . ?
C30 C31 1.398(4) . ?
C31 C32 1.390(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.377(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.394(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 C37 1.509(5) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 Cl1 1.746(11) . ?
C38 Cl2 1.767(10) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.3900 . ?
C39 C44 1.3900 . ?
C39 C45 1.591(18) . ?
C40 C41 1.3900 . ?
C40 H40 0.9500 . ?
C41 C42 1.3900 . ?
C41 H41 0.9500 . ?
C42 C43 1.3900 . ?
C42 H42 0.9500 . ?
C43 C44 1.3900 . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 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
C29 Os N5 76.20(9) . . ?
C29 Os O3 88.85(9) . . ?
N5 Os O3 81.81(8) . . ?
C29 Os C3 90.67(10) . . ?
N5 Os C3 138.80(10) . . ?
O3 Os C3 137.63(10) . . ?
C29 Os C5 133.36(11) . . ?
N5 Os C5 92.87(10) . . ?
O3 Os C5 135.02(10) . . ?
C3 Os C5 68.05(11) . . ?
C29 Os C2 108.36(11) . . ?
N5 Os C2 173.27(10) . . ?
O3 Os C2 102.98(10) . . ?
C3 Os C2 38.06(11) . . ?
C5 Os C2 80.40(11) . . ?
C29 Os C4 100.78(11) . . ?
N5 Os C4 105.25(10) . . ?
O3 Os C4 169.13(9) . . ?
C3 Os C4 38.40(11) . . ?
C5 Os C4 37.98(11) . . ?
C2 Os C4 69.33(11) . . ?
C29 Os C1 143.11(11) . . ?
N5 Os C1 139.23(10) . . ?
O3 Os C1 87.66(10) . . ?
C3 Os C1 68.28(11) . . ?
C5 Os C1 67.69(11) . . ?
C2 Os C1 37.68(11) . . ?
C4 Os C1 81.61(11) . . ?
C29 Os C6 168.82(11) . . ?
N5 Os C6 107.79(10) . . ?
O3 Os C6 101.99(10) . . ?
C3 Os C6 79.49(11) . . ?
C5 Os C6 37.47(11) . . ?
C2 Os C6 66.80(10) . . ?
C4 Os C6 68.18(11) . . ?
C1 Os C6 36.65(10) . . ?
C22 O2 C23 115.2(2) . . ?
C36 O3 Os 125.70(19) . . ?
C11 N5 C17 107.0(2) . . ?
C11 N5 Os 117.90(17) . . ?
C17 N5 Os 134.88(18) . . ?
C11 N8 C12 107.2(2) . . ?
C11 N8 C18 127.7(2) . . ?
C12 N8 C18 124.2(2) . . ?
C6 C1 C2 118.8(3) . . ?
C6 C1 C7 120.7(3) . . ?
C2 C1 C7 120.5(3) . . ?
C6 C1 Os 72.50(16) . . ?
C2 C1 Os 69.07(16) . . ?
C7 C1 Os 127.5(2) . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 Os 69.42(16) . . ?
C1 C2 Os 73.26(16) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
Os C2 H2 129.8 . . ?
C2 C3 C4 122.6(3) . . ?
C2 C3 Os 72.52(17) . . ?
C4 C3 Os 72.71(17) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
Os C3 H3 128.5 . . ?
C5 C4 C3 115.7(3) . . ?
C5 C4 C8 121.2(3) . . ?
C3 C4 C8 123.0(3) . . ?
C5 C4 Os 69.80(16) . . ?
C3 C4 Os 68.89(16) . . ?
C8 C4 Os 131.3(2) . . ?
C4 C5 C6 123.0(3) . . ?
C4 C5 Os 72.22(16) . . ?
C6 C5 Os 75.02(16) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
Os C5 H5 126.2 . . ?
C1 C6 C5 119.5(3) . . ?
C1 C6 Os 70.85(16) . . ?
C5 C6 Os 67.52(15) . . ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
Os C6 H6 134.9 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C4 113.6(3) . . ?
C10 C8 C9 108.7(3) . . ?
C4 C8 C9 112.8(3) . . ?
C10 C8 H8 107.1 . . ?
C4 C8 H8 107.1 . . ?
C9 C8 H8 107.1 . . ?
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 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 N8 110.9(2) . . ?
N5 C11 C24 116.2(2) . . ?
N8 C11 C24 132.9(2) . . ?
N8 C12 C13 131.6(2) . . ?
N8 C12 C17 106.7(2) . . ?
C13 C12 C17 121.7(2) . . ?
C14 C13 C12 117.0(3) . . ?
C14 C13 H13 121.5 . . ?
C12 C13 H13 121.5 . . ?
C13 C14 C15 121.4(3) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C16 C15 C14 121.4(3) . . ?
C16 C15 C22 121.1(3) . . ?
C14 C15 C22 117.5(3) . . ?
C17 C16 C15 117.4(3) . . ?
C17 C16 H16 121.3 . . ?
C15 C16 H16 121.3 . . ?
N5 C17 C16 130.8(3) . . ?
N5 C17 C12 108.1(2) . . ?
C16 C17 C12 121.1(2) . . ?
N8 C18 C19 111.1(2) . . ?
N8 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
N8 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C18 C19 C20 113.1(2) . . ?
C18 C19 H19A 109.0 . . ?
C20 C19 H19A 109.0 . . ?
C18 C19 H19B 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C21 C20 C19 113.4(3) . . ?
C21 C20 H20A 108.9 . . ?
C19 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
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 . . ?
O1 C22 O2 123.0(3) . . ?
O1 C22 C15 124.7(3) . . ?
O2 C22 C15 112.3(2) . . ?
O2 C23 H23A 109.5 . . ?
O2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 121.4(2) . . ?
C25 C24 C11 126.6(2) . . ?
C29 C24 C11 111.9(2) . . ?
C26 C25 C24 119.9(3) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 120.9(2) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C26 C27 C28 118.3(2) . . ?
C26 C27 C30 120.9(2) . . ?
C28 C27 C30 120.8(2) . . ?
C27 C28 C29 122.9(2) . . ?
C27 C28 H28 118.5 . . ?
C29 C28 H28 118.5 . . ?
C28 C29 C24 116.5(2) . . ?
C28 C29 Os 125.9(2) . . ?
C24 C29 Os 117.53(19) . . ?
C35 C30 C31 117.6(3) . . ?
C35 C30 C27 121.1(3) . . ?
C31 C30 C27 121.3(3) . . ?
C32 C31 C30 121.0(3) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C33 C32 C31 120.6(3) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 119.3(3) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C33 C34 C35 120.4(3) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C30 C35 C34 121.1(3) . . ?
C30 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
O4 C36 O3 126.7(3) . . ?
O4 C36 C37 120.3(3) . . ?
O3 C36 C37 112.9(3) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
Cl1 C38 Cl2 112.7(6) . . ?
Cl1 C38 H38A 109.0 . . ?
Cl2 C38 H38A 109.0 . . ?
Cl1 C38 H38B 109.0 . . ?
Cl2 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
C40 C39 C44 120.0 . . ?
C40 C39 C45 111.6(10) . . ?
C44 C39 C45 128.4(10) . . ?
C39 C40 C41 120.0 . . ?
C39 C40 H40 120.0 . . ?
C41 C40 H40 120.0 . . ?
C42 C41 C40 120.0 . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C43 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C42 C43 C44 120.0 . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C39 120.0 . . ?
C43 C44 H44 120.0 . . ?
C39 C44 H44 120.0 . . ?
C39 C45 H45A 109.5 . . ?
C39 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C39 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 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
C6 C1 C2 C3 -1.5(4) . . . . ?
C7 C1 C2 C3 175.3(3) . . . . ?
Os C1 C2 C3 53.2(2) . . . . ?
C6 C1 C2 Os -54.8(2) . . . . ?
C7 C1 C2 Os 122.0(3) . . . . ?
C1 C2 C3 C4 0.1(4) . . . . ?
Os C2 C3 C4 55.2(2) . . . . ?
C1 C2 C3 Os -55.0(2) . . . . ?
C2 C3 C4 C5 -1.7(4) . . . . ?
Os C3 C4 C5 53.3(2) . . . . ?
C2 C3 C4 C8 178.6(3) . . . . ?
Os C3 C4 C8 -126.3(3) . . . . ?
C2 C3 C4 Os -55.1(2) . . . . ?
C3 C4 C5 C6 5.0(4) . . . . ?
C8 C4 C5 C6 -175.4(3) . . . . ?
Os C4 C5 C6 57.8(3) . . . . ?
C3 C4 C5 Os -52.9(2) . . . . ?
C8 C4 C5 Os 126.8(3) . . . . ?
C2 C1 C6 C5 4.5(4) . . . . ?
C7 C1 C6 C5 -172.2(3) . . . . ?
Os C1 C6 C5 -48.6(2) . . . . ?
C2 C1 C6 Os 53.1(2) . . . . ?
C7 C1 C6 Os -123.7(3) . . . . ?
C4 C5 C6 C1 -6.5(4) . . . . ?
Os C5 C6 C1 50.0(2) . . . . ?
C4 C5 C6 Os -56.6(2) . . . . ?
C5 C4 C8 C10 -168.0(3) . . . . ?
C3 C4 C8 C10 11.7(4) . . . . ?
Os C4 C8 C10 -78.3(3) . . . . ?
C5 C4 C8 C9 -43.7(4) . . . . ?
C3 C4 C8 C9 135.9(3) . . . . ?
Os C4 C8 C9 46.0(4) . . . . ?
C17 N5 C11 N8 0.9(3) . . . . ?
Os N5 C11 N8 -174.32(16) . . . . ?
C17 N5 C11 C24 -179.5(2) . . . . ?
Os N5 C11 C24 5.3(3) . . . . ?
C12 N8 C11 N5 -0.6(3) . . . . ?
C18 N8 C11 N5 168.9(2) . . . . ?
C12 N8 C11 C24 179.9(3) . . . . ?
C18 N8 C11 C24 -10.6(5) . . . . ?
C11 N8 C12 C13 179.0(3) . . . . ?
C18 N8 C12 C13 8.9(5) . . . . ?
C11 N8 C12 C17 0.1(3) . . . . ?
C18 N8 C12 C17 -170.0(2) . . . . ?
N8 C12 C13 C14 -179.6(3) . . . . ?
C17 C12 C13 C14 -0.9(4) . . . . ?
C12 C13 C14 C15 0.5(4) . . . . ?
C13 C14 C15 C16 0.1(4) . . . . ?
C13 C14 C15 C22 179.4(3) . . . . ?
C14 C15 C16 C17 -0.4(4) . . . . ?
C22 C15 C16 C17 -179.7(3) . . . . ?
C11 N5 C17 C16 -179.9(3) . . . . ?
Os N5 C17 C16 -5.9(5) . . . . ?
C11 N5 C17 C12 -0.9(3) . . . . ?
Os N5 C17 C12 173.19(19) . . . . ?
C15 C16 C17 N5 179.0(3) . . . . ?
C15 C16 C17 C12 0.0(4) . . . . ?
N8 C12 C17 N5 0.5(3) . . . . ?
C13 C12 C17 N5 -178.6(2) . . . . ?
N8 C12 C17 C16 179.7(2) . . . . ?
C13 C12 C17 C16 0.6(4) . . . . ?
C11 N8 C18 C19 -68.3(3) . . . . ?
C12 N8 C18 C19 99.7(3) . . . . ?
N8 C18 C19 C20 -66.9(3) . . . . ?
C18 C19 C20 C21 173.7(2) . . . . ?
C23 O2 C22 O1 -0.3(4) . . . . ?
C23 O2 C22 C15 -179.4(3) . . . . ?
C16 C15 C22 O1 171.2(3) . . . . ?
C14 C15 C22 O1 -8.2(5) . . . . ?
C16 C15 C22 O2 -9.8(4) . . . . ?
C14 C15 C22 O2 170.8(3) . . . . ?
N5 C11 C24 C25 174.5(3) . . . . ?
N8 C11 C24 C25 -6.0(5) . . . . ?
N5 C11 C24 C29 -1.9(3) . . . . ?
N8 C11 C24 C29 177.6(3) . . . . ?
C29 C24 C25 C26 -1.7(4) . . . . ?
C11 C24 C25 C26 -177.8(3) . . . . ?
C24 C25 C26 C27 -0.1(4) . . . . ?
C25 C26 C27 C28 1.7(4) . . . . ?
C25 C26 C27 C30 -178.9(2) . . . . ?
C26 C27 C28 C29 -1.5(4) . . . . ?
C30 C27 C28 C29 179.1(2) . . . . ?
C27 C28 C29 C24 -0.2(4) . . . . ?
C27 C28 C29 Os -179.4(2) . . . . ?
C25 C24 C29 C28 1.8(4) . . . . ?
C11 C24 C29 C28 178.5(2) . . . . ?
C25 C24 C29 Os -178.9(2) . . . . ?
C11 C24 C29 Os -2.2(3) . . . . ?
C26 C27 C30 C35 -157.3(3) . . . . ?
C28 C27 C30 C35 22.1(4) . . . . ?
C26 C27 C30 C31 23.4(4) . . . . ?
C28 C27 C30 C31 -157.2(3) . . . . ?
C35 C30 C31 C32 -0.2(4) . . . . ?
C27 C30 C31 C32 179.1(3) . . . . ?
C30 C31 C32 C33 -1.0(5) . . . . ?
C31 C32 C33 C34 1.0(5) . . . . ?
C32 C33 C34 C35 0.1(5) . . . . ?
C31 C30 C35 C34 1.3(4) . . . . ?
C27 C30 C35 C34 -178.0(3) . . . . ?
C33 C34 C35 C30 -1.3(5) . . . . ?
Os O3 C36 O4 -11.7(4) . . . . ?
Os O3 C36 C37 167.88(19) . . . . ?
C44 C39 C40 C41 0.0 . . . . ?
C45 C39 C40 C41 -177.8(9) . . . . ?
C39 C40 C41 C42 0.0 . . . . ?
C40 C41 C42 C43 0.0 . . . . ?
C41 C42 C43 C44 0.0 . . . . ?
C42 C43 C44 C39 0.0 . . . . ?
C40 C39 C44 C43 0.0 . . . . ?
C45 C39 C44 C43 177.4(11) . . . . ?

_refine_diff_density_max         2.004
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.121


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methylene chloride, hexane, toluene'
