# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_gabu0528
_database_code_depnum_ccdc_archive 'CCDC 1544885'
_audit_update_record             
;
2017-04-19 deposited with the CCDC.
2017-08-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
cis-[tetrachlorido-bis(1H-indazole)osmate(IV)] acetone solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 Cl4 N4 Os, C3 H6 O'
_chemical_formula_sum            'C17 H18 Cl4 N4 O Os'
_chemical_formula_weight         626.35

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.1258(4)
_cell_length_b                   12.2645(4)
_cell_length_c                   17.8016(4)
_cell_angle_alpha                90
_cell_angle_beta                 131.5370(10)
_cell_angle_gamma                90
_cell_volume                     2145.07(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    199(2)
_cell_measurement_reflns_used    9876
_cell_measurement_theta_min      4.50
_cell_measurement_theta_max      72.30

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    15.943
_shelx_estimated_absorpt_T_min   0.362
_shelx_estimated_absorpt_T_max   0.568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1427
_exptl_absorpt_correction_T_max  0.4480
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      199(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39844
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.901
_diffrn_reflns_theta_max         72.306
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             4212
_reflns_number_gt                4125
_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 Apex2'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0292P)²+2.9312P] 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         4212
_refine_ls_number_parameters     246
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0180
_refine_ls_wR_factor_ref         0.0510
_refine_ls_wR_factor_gt          0.0505
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_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 0.71294(2) 0.05103(2) 0.27590(2) 0.02146(5) Uani 1 1 d . . . . .
Cl1 Cl 0.75844(7) -0.09288(5) 0.37854(5) 0.03590(15) Uani 1 1 d . . . . .
Cl2 Cl 0.65824(7) -0.06915(5) 0.15335(5) 0.03535(15) Uani 1 1 d . . . . .
Cl3 Cl 0.49047(7) 0.06011(6) 0.20642(5) 0.03743(16) Uani 1 1 d . . . . .
Cl4 Cl 0.94016(6) 0.05565(5) 0.35064(5) 0.02699(13) Uani 1 1 d . . . . .
N1 N 0.7584(2) 0.26856(17) 0.21993(15) 0.0274(4) Uani 1 1 d . . . . .
H10 H 0.8314 0.2801 0.2831 0.033 Uiso 1 1 calc R U . . .
N2 N 0.6748(2) 0.18085(17) 0.18534(15) 0.0234(4) Uani 1 1 d . . . . .
C3 C 0.5753(3) 0.1924(2) 0.08629(18) 0.0278(5) Uani 1 1 d . . . . .
H3 H 0.5029 0.1423 0.0434 0.033 Uiso 1 1 calc R U . . .
C4 C 0.5934(3) 0.2892(2) 0.05520(19) 0.0287(5) Uani 1 1 d . . . . .
C5 C 0.5260(3) 0.3409(2) -0.0383(2) 0.0375(6) Uani 1 1 d . . . . .
H5 H 0.4454 0.3109 -0.0988 0.045 Uiso 1 1 calc R U . . .
C6 C 0.5809(4) 0.4356(3) -0.0389(3) 0.0430(8) Uani 1 1 d . . . . .
H6 H 0.5374 0.4717 -0.1008 0.052 Uiso 1 1 calc R U . . .
C7 C 0.7004(4) 0.4804(3) 0.0501(3) 0.0460(8) Uani 1 1 d . . . . .
H7 H 0.7353 0.5460 0.0464 0.055 Uiso 1 1 calc R U . . .
C8 C 0.7682(3) 0.4330(2) 0.1419(3) 0.0423(7) Uani 1 1 d . . . . .
H8 H 0.8484 0.4642 0.2017 0.051 Uiso 1 1 calc R U . . .
C9 C 0.7127(3) 0.3356(2) 0.14285(19) 0.0276(5) Uani 1 1 d . . . . .
N10 N 0.8789(2) 0.14361(17) 0.48424(15) 0.0269(4) Uani 1 1 d . . . . .
H100 H 0.9370 0.0898 0.5063 0.032 Uiso 1 1 calc R U . . .
N11 N 0.7645(2) 0.15883(17) 0.38682(14) 0.0234(4) Uani 1 1 d . . . . .
C12 C 0.7030(2) 0.2473(2) 0.38215(18) 0.0246(5) Uani 1 1 d . . . . .
H12 H 0.6205 0.2764 0.3225 0.030 Uiso 1 1 calc R U . . .
C13 C 0.7779(2) 0.2921(2) 0.47890(18) 0.0231(5) Uani 1 1 d . . . . .
C14 C 0.7635(3) 0.3826(2) 0.5199(2) 0.0297(5) Uani 1 1 d . . . . .
H14 H 0.6877 0.4303 0.4787 0.036 Uiso 1 1 calc R U . . .
C15 C 0.8624(3) 0.3994(2) 0.6211(2) 0.0304(6) Uani 1 1 d . . . . .
H15 H 0.8551 0.4602 0.6504 0.036 Uiso 1 1 calc R U . . .
C16 C 0.9751(3) 0.3286(2) 0.68309(19) 0.0300(5) Uani 1 1 d . . . . .
H16 H 1.0415 0.3436 0.7529 0.036 Uiso 1 1 calc R U . . .
C17 C 0.9921(3) 0.2393(2) 0.64635(18) 0.0295(5) Uani 1 1 d . . . . .
H17 H 1.0677 0.1917 0.6886 0.035 Uiso 1 1 calc R U . . .
C18 C 0.8911(2) 0.22234(19) 0.54237(18) 0.0239(5) Uani 1 1 d . . . . .
O1 O 0.9625(2) 0.3440(2) 0.41092(17) 0.0532(6) Uani 1 1 d . . . . .
C19 C 1.0856(3) 0.3498(2) 0.4772(2) 0.0360(6) Uani 1 1 d . . . . .
C20 C 1.1473(3) 0.3966(3) 0.5768(2) 0.0407(7) Uani 1 1 d . . . . .
H20A H 1.0754 0.4131 0.5780 0.061 Uiso 1 1 calc R U . . .
H20B H 1.1964 0.4637 0.5882 0.061 Uiso 1 1 calc R U . . .
H20C H 1.2108 0.3438 0.6297 0.061 Uiso 1 1 calc R U . . .
C21 C 1.1792(4) 0.3114(3) 0.4623(3) 0.0449(7) Uani 1 1 d . . . . .
H21A H 1.2331 0.2497 0.5072 0.067 Uiso 1 1 calc R U . . .
H21B H 1.2403 0.3709 0.4776 0.067 Uiso 1 1 calc R U . . .
H21C H 1.1256 0.2883 0.3925 0.067 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
Os N2 2.077(2) . ?
Os N11 2.082(2) . ?
Os Cl3 2.2976(7) . ?
Os Cl1 2.3158(6) . ?
Os Cl2 2.3174(6) . ?
Os Cl4 2.3251(6) . ?
N1 C9 1.351(3) . ?
N1 N2 1.358(3) . ?
N1 H10 0.8800 . ?
N2 C3 1.335(3) . ?
C3 C4 1.395(4) . ?
C3 H3 0.9500 . ?
C4 C9 1.403(4) . ?
C4 C5 1.416(4) . ?
C5 C6 1.370(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.406(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.368(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.405(4) . ?
C8 H8 0.9500 . ?
N10 C18 1.345(3) . ?
N10 N11 1.358(3) . ?
N10 H100 0.8800 . ?
N11 C12 1.322(3) . ?
C12 C13 1.410(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.409(4) . ?
C13 C18 1.411(3) . ?
C14 C15 1.367(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.413(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.368(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.405(3) . ?
C17 H17 0.9500 . ?
O1 C19 1.216(4) . ?
C19 C20 1.491(4) . ?
C19 C21 1.495(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 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
N2 Os N11 90.51(8) . . ?
N2 Os Cl3 88.80(6) . . ?
N11 Os Cl3 88.71(6) . . ?
N2 Os Cl1 179.22(6) . . ?
N11 Os Cl1 89.09(6) . . ?
Cl3 Os Cl1 91.86(3) . . ?
N2 Os Cl2 89.54(6) . . ?
N11 Os Cl2 179.33(6) . . ?
Cl3 Os Cl2 91.97(3) . . ?
Cl1 Os Cl2 90.85(2) . . ?
N2 Os Cl4 89.01(6) . . ?
N11 Os Cl4 87.42(6) . . ?
Cl3 Os Cl4 175.54(2) . . ?
Cl1 Os Cl4 90.30(2) . . ?
Cl2 Os Cl4 91.91(2) . . ?
C9 N1 N2 109.9(2) . . ?
C9 N1 H10 125.1 . . ?
N2 N1 H10 125.1 . . ?
C3 N2 N1 107.7(2) . . ?
C3 N2 Os 128.89(17) . . ?
N1 N2 Os 123.30(15) . . ?
N2 C3 C4 109.8(2) . . ?
N2 C3 H3 125.1 . . ?
C4 C3 H3 125.1 . . ?
C3 C4 C9 105.2(2) . . ?
C3 C4 C5 135.2(3) . . ?
C9 C4 C5 119.5(3) . . ?
C6 C5 C4 117.8(3) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
C5 C6 C7 121.5(3) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C6 122.4(3) . . ?
C8 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
C7 C8 C9 116.4(3) . . ?
C7 C8 H8 121.8 . . ?
C9 C8 H8 121.8 . . ?
N1 C9 C4 107.4(2) . . ?
N1 C9 C8 130.2(3) . . ?
C4 C9 C8 122.4(3) . . ?
C18 N10 N11 110.5(2) . . ?
C18 N10 H100 124.7 . . ?
N11 N10 H100 124.7 . . ?
C12 N11 N10 107.8(2) . . ?
C12 N11 Os 131.38(16) . . ?
N10 N11 Os 120.83(16) . . ?
N11 C12 C13 109.9(2) . . ?
N11 C12 H12 125.0 . . ?
C13 C12 H12 125.0 . . ?
C14 C13 C12 135.7(2) . . ?
C14 C13 C18 119.7(2) . . ?
C12 C13 C18 104.7(2) . . ?
C15 C14 C13 117.7(2) . . ?
C15 C14 H14 121.2 . . ?
C13 C14 H14 121.2 . . ?
C14 C15 C16 121.6(2) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C17 C16 C15 122.5(2) . . ?
C17 C16 H16 118.8 . . ?
C15 C16 H16 118.8 . . ?
C16 C17 C18 116.0(2) . . ?
C16 C17 H17 122.0 . . ?
C18 C17 H17 122.0 . . ?
N10 C18 C17 130.3(2) . . ?
N10 C18 C13 107.1(2) . . ?
C17 C18 C13 122.5(2) . . ?
O1 C19 C20 120.1(3) . . ?
O1 C19 C21 121.9(3) . . ?
C20 C19 C21 118.0(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 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
C9 N1 N2 C3 -0.5(3) . . . . ?
C9 N1 N2 Os 175.60(16) . . . . ?
N1 N2 C3 C4 -0.1(3) . . . . ?
Os N2 C3 C4 -175.90(17) . . . . ?
N2 C3 C4 C9 0.6(3) . . . . ?
N2 C3 C4 C5 176.7(3) . . . . ?
C3 C4 C5 C6 -176.0(3) . . . . ?
C9 C4 C5 C6 -0.3(4) . . . . ?
C4 C5 C6 C7 0.1(4) . . . . ?
C5 C6 C7 C8 -0.2(5) . . . . ?
C6 C7 C8 C9 0.5(5) . . . . ?
N2 N1 C9 C4 0.9(3) . . . . ?
N2 N1 C9 C8 -177.4(3) . . . . ?
C3 C4 C9 N1 -0.9(3) . . . . ?
C5 C4 C9 N1 -177.7(2) . . . . ?
C3 C4 C9 C8 177.5(3) . . . . ?
C5 C4 C9 C8 0.7(4) . . . . ?
C7 C8 C9 N1 177.2(3) . . . . ?
C7 C8 C9 C4 -0.8(4) . . . . ?
C18 N10 N11 C12 0.0(3) . . . . ?
C18 N10 N11 Os -179.59(16) . . . . ?
N10 N11 C12 C13 -0.2(3) . . . . ?
Os N11 C12 C13 179.35(17) . . . . ?
N11 C12 C13 C14 -179.7(3) . . . . ?
N11 C12 C13 C18 0.3(3) . . . . ?
C12 C13 C14 C15 -179.4(3) . . . . ?
C18 C13 C14 C15 0.6(4) . . . . ?
C13 C14 C15 C16 -0.4(4) . . . . ?
C14 C15 C16 C17 -0.2(4) . . . . ?
C15 C16 C17 C18 0.6(4) . . . . ?
N11 N10 C18 C17 -180.0(3) . . . . ?
N11 N10 C18 C13 0.2(3) . . . . ?
C16 C17 C18 N10 179.7(3) . . . . ?
C16 C17 C18 C13 -0.4(4) . . . . ?
C14 C13 C18 N10 179.7(2) . . . . ?
C12 C13 C18 N10 -0.3(3) . . . . ?
C14 C13 C18 C17 -0.2(4) . . . . ?
C12 C13 C18 C17 179.8(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H10 O1 0.88 1.89 2.741(3) 163.3 .
C3 H3 Cl2 0.95 2.78 3.541(3) 137.9 3_655
N10 H100 Cl4 0.88 2.61 3.316(2) 137.6 3_756

_refine_diff_density_max         0.417
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.097

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_gabu372
_database_code_depnum_ccdc_archive 'CCDC 1544886'
_audit_update_record             
;
2017-04-19 deposited with the CCDC.
2017-08-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
trans-[Dichlorido-bis(1H-indazole)osmate(IV)]didimethylsulfoxide solvate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 Cl4 N4 Os, 2(C2 H6 O S)'
_chemical_formula_sum            'C18 H24 Cl4 N4 O2 Os S2'
_chemical_formula_weight         724.53

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'
S S 0.1246 0.1234 '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                   10.2354(6)
_cell_length_b                   14.3781(6)
_cell_length_c                   16.4733(9)
_cell_angle_alpha                90
_cell_angle_beta                 91.046(2)
_cell_angle_gamma                90
_cell_volume                     2423.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      28.68

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_F_000             1408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    5.898
_shelx_estimated_absorpt_T_min   0.590
_shelx_estimated_absorpt_T_max   0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5900
_exptl_absorpt_correction_T_max  0.8911
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            85723
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_av_R_equivalents  0.1041
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.324
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5247
_reflns_number_gt                3988
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0175P)²+1.5366P] 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         5247
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0579
_refine_ls_wR_factor_gt          0.0530
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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 0.61928(2) 0.74747(2) 0.99380(2) 0.01294(6) Uani 1 1 d . . . . .
Cl1 Cl 0.66693(9) 0.59237(6) 0.97621(5) 0.01891(19) Uani 1 1 d . . . . .
Cl2 Cl 0.69064(9) 0.73755(6) 1.12814(5) 0.01924(19) Uani 1 1 d . . . . .
Cl3 Cl 0.57593(9) 0.90336(6) 1.01390(5) 0.0215(2) Uani 1 1 d . . . . .
Cl4 Cl 0.54705(9) 0.75772(6) 0.85980(5) 0.0195(2) Uani 1 1 d . . . . .
N1 N 0.8652(3) 0.74790(17) 0.89342(18) 0.0171(7) Uani 1 1 d . . . . .
H10 H 0.8302 0.7081 0.8588 0.021 Uiso 1 1 calc R U . . .
N2 N 0.8055(3) 0.78317(19) 0.95955(17) 0.0154(6) Uani 1 1 d . . . . .
C3 C 0.8875(3) 0.8416(2) 0.9964(2) 0.0195(8) Uani 1 1 d . . . . .
H3 H 0.8690 0.8758 1.0441 0.023 Uiso 1 1 calc R U . . .
C4 C 1.0051(3) 0.8455(2) 0.9548(2) 0.0179(8) Uani 1 1 d . . . . .
C5 C 1.1269(3) 0.8901(2) 0.9666(2) 0.0209(8) Uani 1 1 d . . . . .
H5 H 1.1409 0.9317 1.0107 0.025 Uiso 1 1 calc R U . . .
C6 C 1.2227(4) 0.8723(3) 0.9138(2) 0.0244(9) Uani 1 1 d . . . . .
H6 H 1.3053 0.9014 0.9214 0.029 Uiso 1 1 calc R U . . .
C7 C 1.2030(4) 0.8109(3) 0.8471(2) 0.0241(9) Uani 1 1 d . . . . .
H7 H 1.2726 0.8003 0.8108 0.029 Uiso 1 1 calc R U . . .
C8 C 1.0862(4) 0.7666(2) 0.8339(2) 0.0192(8) Uani 1 1 d . . . . .
H8 H 1.0728 0.7259 0.7891 0.023 Uiso 1 1 calc R U . . .
C9 C 0.9881(3) 0.7840(2) 0.8892(2) 0.0151(8) Uani 1 1 d . . . . .
N10 N 0.3469(3) 0.66270(18) 0.99009(17) 0.0159(6) Uani 1 1 d . . . . .
H100 H 0.3626 0.6333 0.9444 0.019 Uiso 1 1 calc R U . . .
N11 N 0.4334(3) 0.71713(19) 1.03082(17) 0.0151(6) Uani 1 1 d . . . . .
C12 C 0.3757(4) 0.7495(2) 1.0971(2) 0.0169(8) Uani 1 1 d . . . . .
H12 H 0.4151 0.7897 1.1363 0.020 Uiso 1 1 calc R U . . .
C13 C 0.2487(3) 0.7152(2) 1.0997(2) 0.0161(8) Uani 1 1 d . . . . .
C14 C 0.1435(4) 0.7269(2) 1.1533(2) 0.0174(8) Uani 1 1 d . . . . .
H14 H 0.1526 0.7635 1.2011 0.021 Uiso 1 1 calc R U . . .
C15 C 0.0294(4) 0.6839(2) 1.1338(2) 0.0213(8) Uani 1 1 d . . . . .
H15 H -0.0427 0.6916 1.1687 0.026 Uiso 1 1 calc R U . . .
C16 C 0.0136(4) 0.6282(2) 1.0637(2) 0.0205(8) Uani 1 1 d . . . . .
H16 H -0.0683 0.5992 1.0527 0.025 Uiso 1 1 calc R U . . .
C17 C 0.1138(3) 0.6153(2) 1.0114(2) 0.0185(8) Uani 1 1 d . . . . .
H17 H 0.1039 0.5776 0.9643 0.022 Uiso 1 1 calc R U . . .
C18 C 0.2319(3) 0.6600(2) 1.03018(19) 0.0143(7) Uani 1 1 d . . . . .
S1 S 0.84565(9) 0.52497(6) 0.76516(6) 0.0215(2) Uani 1 1 d . . . . .
O1 O 0.8270(2) 0.62919(16) 0.76784(14) 0.0256(6) Uani 1 1 d . . . . .
C19 C 0.7747(4) 0.4894(3) 0.6705(2) 0.0332(10) Uani 1 1 d . . . . .
H19A H 0.7834 0.4218 0.6647 0.050 Uiso 1 1 calc R U . . .
H19B H 0.6819 0.5063 0.6687 0.050 Uiso 1 1 calc R U . . .
H19C H 0.8197 0.5204 0.6260 0.050 Uiso 1 1 calc R U . . .
C20 C 1.0122(3) 0.5076(3) 0.7392(2) 0.0274(9) Uani 1 1 d . . . . .
H20A H 1.0305 0.4408 0.7365 0.041 Uiso 1 1 calc R U . . .
H20B H 1.0284 0.5361 0.6863 0.041 Uiso 1 1 calc R U . . .
H20C H 1.0691 0.5363 0.7806 0.041 Uiso 1 1 calc R U . . .
S2 S 0.34331(9) 0.49994(6) 0.79233(5) 0.0202(2) Uani 1 1 d . . . . .
O2 O 0.2953(2) 0.56994(16) 0.85227(14) 0.0249(6) Uani 1 1 d . . . . .
C21 C 0.3936(4) 0.5663(3) 0.7074(2) 0.0317(10) Uani 1 1 d . . . . .
H21A H 0.4265 0.5245 0.6654 0.048 Uiso 1 1 calc R U . . .
H21B H 0.3191 0.6016 0.6855 0.048 Uiso 1 1 calc R U . . .
H21C H 0.4631 0.6094 0.7244 0.048 Uiso 1 1 calc R U . . .
C22 C 0.5009(3) 0.4643(3) 0.8263(2) 0.0225(8) Uani 1 1 d . . . . .
H22A H 0.5357 0.4183 0.7885 0.034 Uiso 1 1 calc R U . . .
H22B H 0.5592 0.5184 0.8287 0.034 Uiso 1 1 calc R U . . .
H22C H 0.4949 0.4366 0.8804 0.034 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os N11 2.055(3) . ?
Os N2 2.063(3) . ?
Os Cl1 2.3022(8) . ?
Os Cl3 2.3099(8) . ?
Os Cl4 2.3197(9) . ?
Os Cl2 2.3222(9) . ?
N1 N2 1.357(4) . ?
N1 C9 1.363(4) . ?
N1 H10 0.8800 . ?
N2 C3 1.327(4) . ?
C3 C4 1.397(5) . ?
C3 H3 0.9500 . ?
C4 C9 1.404(5) . ?
C4 C5 1.412(5) . ?
C5 C6 1.347(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.421(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.368(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.391(5) . ?
C8 H8 0.9500 . ?
N10 N11 1.351(4) . ?
N10 C18 1.361(4) . ?
N10 H100 0.8800 . ?
N11 C12 1.334(4) . ?
C12 C13 1.393(5) . ?
C12 H12 0.9500 . ?
C13 C18 1.401(5) . ?
C13 C14 1.415(5) . ?
C14 C15 1.354(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.413(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.364(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.399(5) . ?
C17 H17 0.9500 . ?
S1 O1 1.511(3) . ?
S1 C20 1.782(4) . ?
S1 C19 1.783(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
S2 O2 1.499(2) . ?
S2 C22 1.773(4) . ?
S2 C21 1.778(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 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
N11 Os N2 177.52(10) . . ?
N11 Os Cl1 91.78(8) . . ?
N2 Os Cl1 90.44(8) . . ?
N11 Os Cl3 88.98(8) . . ?
N2 Os Cl3 88.78(8) . . ?
Cl1 Os Cl3 178.50(3) . . ?
N11 Os Cl4 90.87(8) . . ?
N2 Os Cl4 90.23(8) . . ?
Cl1 Os Cl4 90.36(3) . . ?
Cl3 Os Cl4 90.92(3) . . ?
N11 Os Cl2 88.91(8) . . ?
N2 Os Cl2 89.99(8) . . ?
Cl1 Os Cl2 89.82(3) . . ?
Cl3 Os Cl2 88.91(3) . . ?
Cl4 Os Cl2 179.72(3) . . ?
N2 N1 C9 109.2(3) . . ?
N2 N1 H10 125.4 . . ?
C9 N1 H10 125.4 . . ?
C3 N2 N1 108.3(3) . . ?
C3 N2 Os 127.8(2) . . ?
N1 N2 Os 124.0(2) . . ?
N2 C3 C4 110.1(3) . . ?
N2 C3 H3 124.9 . . ?
C4 C3 H3 124.9 . . ?
C3 C4 C9 104.9(3) . . ?
C3 C4 C5 135.7(3) . . ?
C9 C4 C5 119.3(3) . . ?
C6 C5 C4 118.3(3) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
C5 C6 C7 121.6(3) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C6 121.5(4) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C7 C8 C9 116.9(3) . . ?
C7 C8 H8 121.6 . . ?
C9 C8 H8 121.6 . . ?
N1 C9 C8 130.0(3) . . ?
N1 C9 C4 107.6(3) . . ?
C8 C9 C4 122.4(3) . . ?
N11 N10 C18 109.9(3) . . ?
N11 N10 H100 125.0 . . ?
C18 N10 H100 125.0 . . ?
C12 N11 N10 108.2(3) . . ?
C12 N11 Os 126.5(2) . . ?
N10 N11 Os 125.3(2) . . ?
N11 C12 C13 109.2(3) . . ?
N11 C12 H12 125.4 . . ?
C13 C12 H12 125.4 . . ?
C12 C13 C18 106.0(3) . . ?
C12 C13 C14 134.3(3) . . ?
C18 C13 C14 119.6(3) . . ?
C15 C14 C13 117.4(3) . . ?
C15 C14 H14 121.3 . . ?
C13 C14 H14 121.3 . . ?
C14 C15 C16 122.5(3) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
C17 C16 C15 121.1(3) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 117.0(3) . . ?
C16 C17 H17 121.5 . . ?
C18 C17 H17 121.5 . . ?
N10 C18 C17 131.1(3) . . ?
N10 C18 C13 106.7(3) . . ?
C17 C18 C13 122.2(3) . . ?
O1 S1 C20 105.53(17) . . ?
O1 S1 C19 105.11(17) . . ?
C20 S1 C19 97.23(19) . . ?
S1 C19 H19A 109.5 . . ?
S1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
S1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
S1 C20 H20A 109.5 . . ?
S1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
S1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 S2 C22 107.07(16) . . ?
O2 S2 C21 105.15(17) . . ?
C22 S2 C21 97.37(19) . . ?
S2 C21 H21A 109.5 . . ?
S2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
S2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
S2 C22 H22A 109.5 . . ?
S2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
S2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 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
C9 N1 N2 C3 0.8(4) . . . . ?
C9 N1 N2 Os -178.6(2) . . . . ?
N1 N2 C3 C4 -0.4(4) . . . . ?
Os N2 C3 C4 178.9(2) . . . . ?
N2 C3 C4 C9 -0.1(4) . . . . ?
N2 C3 C4 C5 -176.4(4) . . . . ?
C3 C4 C5 C6 176.2(4) . . . . ?
C9 C4 C5 C6 0.3(5) . . . . ?
C4 C5 C6 C7 0.6(5) . . . . ?
C5 C6 C7 C8 -0.5(6) . . . . ?
C6 C7 C8 C9 -0.4(5) . . . . ?
N2 N1 C9 C8 178.0(3) . . . . ?
N2 N1 C9 C4 -0.9(4) . . . . ?
C7 C8 C9 N1 -177.3(3) . . . . ?
C7 C8 C9 C4 1.4(5) . . . . ?
C3 C4 C9 N1 0.6(4) . . . . ?
C5 C4 C9 N1 177.6(3) . . . . ?
C3 C4 C9 C8 -178.4(3) . . . . ?
C5 C4 C9 C8 -1.4(5) . . . . ?
C18 N10 N11 C12 0.2(4) . . . . ?
C18 N10 N11 Os -177.9(2) . . . . ?
N10 N11 C12 C13 0.1(4) . . . . ?
Os N11 C12 C13 178.2(2) . . . . ?
N11 C12 C13 C18 -0.4(4) . . . . ?
N11 C12 C13 C14 -178.6(4) . . . . ?
C12 C13 C14 C15 177.4(4) . . . . ?
C18 C13 C14 C15 -0.6(5) . . . . ?
C13 C14 C15 C16 0.8(5) . . . . ?
C14 C15 C16 C17 -0.3(5) . . . . ?
C15 C16 C17 C18 -0.4(5) . . . . ?
N11 N10 C18 C17 178.6(3) . . . . ?
N11 N10 C18 C13 -0.4(4) . . . . ?
C16 C17 C18 N10 -178.3(3) . . . . ?
C16 C17 C18 C13 0.6(5) . . . . ?
C12 C13 C18 N10 0.5(4) . . . . ?
C14 C13 C18 N10 179.0(3) . . . . ?
C12 C13 C18 C17 -178.6(3) . . . . ?
C14 C13 C18 C17 -0.1(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H10 O1 0.88 1.88 2.705(4) 155.6 .
C8 H8 Cl2 0.95 2.98 3.573(4) 121.8 4_675
N10 H100 O2 0.88 1.89 2.677(4) 148.1 .
C12 H12 O1 0.95 2.64 3.355(4) 132.9 4_576
C19 H19A Cl4 0.98 2.96 3.835(4) 149.0 2_646
C20 H20C S2 0.98 2.86 3.487(4) 122.7 1_655
C20 H20C O2 0.98 2.62 3.532(5) 154.0 1_655
C21 H21B Cl2 0.98 2.81 3.725(4) 154.9 4_575
C22 H22B Cl1 0.98 2.86 3.496(4) 123.8 .
C22 H22C Cl1 0.98 2.94 3.795(4) 146.5 3_667

_refine_diff_density_max         1.472
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.142

_shelxl_version_number           2014-3

