# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1ClO4
_database_code_depnum_ccdc_archive 'CCDC 1465137'
_audit_update_record             
;
2016-03-12 deposited with the CCDC.
2016-10-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H29 Cl N4 O6 Os'
_chemical_formula_weight         875.35

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.694(3)
_cell_length_b                   12.469(4)
_cell_length_c                   13.505(4)
_cell_angle_alpha                110.800(3)
_cell_angle_beta                 97.5790(10)
_cell_angle_gamma                112.346(3)
_cell_volume                     1619.5(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6089
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      29.3

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             804
_exptl_absorpt_coefficient_mu    4.072
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4293
_exptl_absorpt_correction_T_max  0.9604
_exptl_absorpt_process_details   
'(a) Busing, W. R.; Levy, H. A. Acta Crystallogr. 1957, 10, 180-182. (b) Coppens, P.; Leiserowitz, L.; Rabinovich, D. Acta Crystallogr. 1965, 18, 1035-1038'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11713
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5606
_reflns_number_gt                5245
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  ORTEP

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0327P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5606
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0668
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.205464(16) 0.260097(14) 0.479462(13) 0.01754(7) Uani 1 1 d . . .
Cl1 Cl 0.00666(11) 0.28409(10) 0.09438(9) 0.0270(3) Uani 1 1 d . . .
O2 O 0.2191(3) 0.1015(3) 0.4791(2) 0.0200(6) Uani 1 1 d . . .
O1 O 0.3738(3) 0.3782(3) 0.6085(2) 0.0213(7) Uani 1 1 d . . .
O3 O 0.1233(3) 0.2712(3) 0.0989(3) 0.0439(9) Uani 1 1 d . . .
O6 O -0.0185(5) 0.3028(4) 0.1986(3) 0.0595(12) Uani 1 1 d . . .
O5 O 0.0158(4) 0.3886(3) 0.0707(3) 0.0503(10) Uani 1 1 d . . .
O4 O -0.0998(4) 0.1657(3) 0.0108(3) 0.0587(12) Uani 1 1 d . . .
N4 N 0.1155(3) 0.2826(3) 0.6002(3) 0.0176(8) Uani 1 1 d . . .
N3 N 0.1892(3) 0.4196(3) 0.4941(3) 0.0176(8) Uani 1 1 d . . .
N2 N 0.0523(3) 0.1352(3) 0.3411(3) 0.0186(8) Uani 1 1 d . . .
N1 N 0.2957(3) 0.2446(3) 0.3597(3) 0.0181(8) Uani 1 1 d . . .
C33 C 0.0689(4) 0.1990(4) 0.6444(4) 0.0246(10) Uani 1 1 d . . .
H33 H 0.0634 0.1155 0.6101 0.029 Uiso 1 1 calc R . .
C32 C 0.0293(5) 0.2314(4) 0.7373(4) 0.0290(11) Uani 1 1 d . . .
H32 H -0.0017 0.1713 0.7672 0.035 Uiso 1 1 calc R . .
C31 C 0.0345(5) 0.3518(4) 0.7873(4) 0.0283(11) Uani 1 1 d . . .
H31 H 0.0097 0.3763 0.8528 0.034 Uiso 1 1 calc R . .
C30 C 0.0769(4) 0.4358(4) 0.7399(4) 0.0288(11) Uani 1 1 d . . .
H30 H 0.0794 0.5183 0.7719 0.035 Uiso 1 1 calc R . .
C29 C 0.1156(4) 0.3997(4) 0.6458(3) 0.0194(9) Uani 1 1 d . . .
C28 C 0.1547(4) 0.4763(4) 0.5850(3) 0.0200(9) Uani 1 1 d . . .
C27 C 0.1504(4) 0.5925(4) 0.6092(4) 0.0238(10) Uani 1 1 d . . .
H27 H 0.1284 0.6314 0.6731 0.029 Uiso 1 1 calc R . .
C26 C 0.1782(4) 0.6503(4) 0.5402(4) 0.0281(11) Uani 1 1 d . . .
H26 H 0.1762 0.7301 0.5563 0.034 Uiso 1 1 calc R . .
C25 C 0.2094(4) 0.5917(4) 0.4462(4) 0.0262(10) Uani 1 1 d . . .
H25 H 0.2273 0.6301 0.3969 0.031 Uiso 1 1 calc R . .
C24 C 0.2139(4) 0.4788(4) 0.4261(4) 0.0251(10) Uani 1 1 d . . .
H24 H 0.2351 0.4394 0.3619 0.030 Uiso 1 1 calc R . .
C23 C -0.0742(4) 0.0835(4) 0.3373(4) 0.0210(9) Uani 1 1 d . . .
H23 H -0.0951 0.1134 0.4041 0.025 Uiso 1 1 calc R . .
C22 C -0.1731(4) -0.0094(4) 0.2421(4) 0.0266(10) Uani 1 1 d . . .
H22 H -0.2602 -0.0435 0.2438 0.032 Uiso 1 1 calc R . .
C21 C -0.1455(4) -0.0541(4) 0.1423(4) 0.0251(10) Uani 1 1 d . . .
H21 H -0.2129 -0.1184 0.0750 0.030 Uiso 1 1 calc R . .
C20 C -0.0177(4) -0.0023(4) 0.1444(4) 0.0242(10) Uani 1 1 d . . .
H20 H 0.0039 -0.0313 0.0778 0.029 Uiso 1 1 calc R . .
C19 C 0.0803(4) 0.0923(4) 0.2432(3) 0.0193(9) Uani 1 1 d . . .
C18 C 0.2180(4) 0.1531(4) 0.2539(3) 0.0181(9) Uani 1 1 d . . .
C17 C 0.2700(4) 0.1269(4) 0.1668(4) 0.0224(10) Uani 1 1 d . . .
H17 H 0.2150 0.0633 0.0939 0.027 Uiso 1 1 calc R . .
C16 C 0.4021(4) 0.1938(4) 0.1866(4) 0.0262(10) Uani 1 1 d . . .
H16 H 0.4392 0.1753 0.1281 0.031 Uiso 1 1 calc R . .
C15 C 0.4795(4) 0.2882(4) 0.2927(4) 0.0254(10) Uani 1 1 d . . .
H15 H 0.5702 0.3369 0.3075 0.030 Uiso 1 1 calc R . .
C14 C 0.4245(4) 0.3111(4) 0.3766(4) 0.0239(10) Uani 1 1 d . . .
H14 H 0.4787 0.3761 0.4492 0.029 Uiso 1 1 calc R . .
C10 C 0.3036(4) -0.0249(4) 0.5151(4) 0.0234(10) Uani 1 1 d . . .
H10 H 0.2296 -0.0992 0.4586 0.028 Uiso 1 1 calc R . .
C9 C 0.3967(5) -0.0396(4) 0.5705(4) 0.0270(11) Uani 1 1 d . . .
H9 H 0.3870 -0.1244 0.5505 0.032 Uiso 1 1 calc R . .
C8 C 0.5086(4) 0.0662(4) 0.6577(4) 0.0253(10) Uani 1 1 d . . .
C7 C 0.6061(5) 0.0507(5) 0.7127(4) 0.0348(12) Uani 1 1 d . . .
H7 H 0.5976 -0.0338 0.6922 0.042 Uiso 1 1 calc R . .
C6 C 0.7136(5) 0.1536(5) 0.7952(4) 0.0377(12) Uani 1 1 d . . .
H6 H 0.7788 0.1408 0.8320 0.045 Uiso 1 1 calc R . .
C5 C 0.7268(5) 0.2768(5) 0.8248(4) 0.0355(12) Uani 1 1 d . . .
H5 H 0.8003 0.3483 0.8839 0.043 Uiso 1 1 calc R . .
C4 C 0.6341(4) 0.2984(4) 0.7693(4) 0.0274(11) Uani 1 1 d . . .
C3 C 0.6495(5) 0.4254(4) 0.7982(4) 0.0272(11) Uani 1 1 d . . .
H3 H 0.7231 0.4965 0.8575 0.033 Uiso 1 1 calc R . .
C2 C 0.5625(4) 0.4479(4) 0.7439(4) 0.0261(10) Uani 1 1 d . . .
H2 H 0.5773 0.5343 0.7644 0.031 Uiso 1 1 calc R . .
C1 C 0.4482(4) 0.3439(4) 0.6560(3) 0.0187(9) Uani 1 1 d . . .
C12 C 0.4262(4) 0.2116(4) 0.6258(3) 0.0194(9) Uani 1 1 d . . .
C11 C 0.3139(4) 0.1010(4) 0.5396(3) 0.0192(9) Uani 1 1 d . . .
C13 C 0.5222(4) 0.1926(4) 0.6838(3) 0.0219(10) Uani 1 1 d . . .
C34 C 0.5898(5) 0.4733(5) 0.0516(4) 0.0429(13) Uani 1 1 d . . .
H34 H 0.6512 0.4556 0.0873 0.052 Uiso 1 1 calc R . .
C35 C 0.6200(6) 0.5974(5) 0.0672(5) 0.0463(14) Uani 1 1 d . . .
H35 H 0.7036 0.6659 0.1137 0.056 Uiso 1 1 calc R . .
C36 C 0.5309(6) 0.6238(5) 0.0165(5) 0.0449(14) Uani 1 1 d . . .
H36 H 0.5534 0.7102 0.0290 0.054 Uiso 1 1 calc R . .
C37 C 0.5199(5) 0.9531(5) 0.0751(4) 0.0394(13) Uani 1 1 d . . .
H37 H 0.5332 0.9199 0.1265 0.047 Uiso 1 1 calc R . .
C38 C 0.3997(5) 0.8931(5) -0.0049(4) 0.0374(13) Uani 1 1 d . . .
H38 H 0.3311 0.8196 -0.0069 0.045 Uiso 1 1 calc R . .
C39 C 0.3784(5) 0.9372(5) -0.0800(4) 0.0390(13) Uani 1 1 d . . .
H39 H 0.2961 0.8947 -0.1350 0.047 Uiso 1 1 calc R . .


_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 N3 2.012(3) . ?
Os1 N2 2.014(4) . ?
Os1 N1 2.037(3) . ?
Os1 O1 2.037(3) . ?
Os1 O2 2.042(3) . ?
Os1 N4 2.048(3) . ?
Cl1 O5 1.418(4) . ?
Cl1 O3 1.429(3) . ?
Cl1 O4 1.432(4) . ?
Cl1 O6 1.432(4) . ?
O2 C11 1.292(5) . ?
O1 C1 1.297(5) . ?
N4 C33 1.355(5) . ?
N4 C29 1.367(5) . ?
N3 C24 1.364(5) . ?
N3 C28 1.378(5) . ?
N2 C23 1.356(5) . ?
N2 C19 1.373(5) . ?
N1 C14 1.353(5) . ?
N1 C18 1.371(5) . ?
C33 C32 1.375(6) . ?
C33 H33 0.9500 . ?
C32 C31 1.382(6) . ?
C32 H32 0.9500 . ?
C31 C30 1.385(6) . ?
C31 H31 0.9500 . ?
C30 C29 1.387(6) . ?
C30 H30 0.9500 . ?
C29 C28 1.457(6) . ?
C28 C27 1.390(5) . ?
C27 C26 1.368(6) . ?
C27 H27 0.9500 . ?
C26 C25 1.396(6) . ?
C26 H26 0.9500 . ?
C25 C24 1.359(6) . ?
C25 H25 0.9500 . ?
C24 H24 0.9500 . ?
C23 C22 1.365(6) . ?
C23 H23 0.9500 . ?
C22 C21 1.397(6) . ?
C22 H22 0.9500 . ?
C21 C20 1.376(6) . ?
C21 H21 0.9500 . ?
C20 C19 1.391(6) . ?
C20 H20 0.9500 . ?
C19 C18 1.457(6) . ?
C18 C17 1.389(5) . ?
C17 C16 1.380(6) . ?
C17 H17 0.9500 . ?
C16 C15 1.382(6) . ?
C16 H16 0.9500 . ?
C15 C14 1.371(6) . ?
C15 H15 0.9500 . ?
C14 H14 0.9500 . ?
C10 C9 1.347(6) . ?
C10 C11 1.436(6) . ?
C10 H10 0.9500 . ?
C9 C8 1.420(6) . ?
C9 H9 0.9500 . ?
C8 C7 1.391(7) . ?
C8 C13 1.426(6) . ?
C7 C6 1.362(7) . ?
C7 H7 0.9500 . ?
C6 C5 1.382(7) . ?
C6 H6 0.9500 . ?
C5 C4 1.399(6) . ?
C5 H5 0.9500 . ?
C4 C13 1.412(6) . ?
C4 C3 1.421(6) . ?
C3 C2 1.348(6) . ?
C3 H3 0.9500 . ?
C2 C1 1.431(6) . ?
C2 H2 0.9500 . ?
C1 C12 1.458(6) . ?
C12 C13 1.425(6) . ?
C12 C11 1.435(6) . ?
C34 C36 1.368(8) 2_665 ?
C34 C35 1.377(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.376(8) . ?
C35 H35 0.9500 . ?
C36 C34 1.368(8) 2_665 ?
C36 H36 0.9500 . ?
C37 C38 1.388(7) . ?
C37 C39 1.403(7) 2_675 ?
C37 H37 0.9500 . ?
C38 C39 1.351(7) . ?
C38 H38 0.9500 . ?
C39 C37 1.403(7) 2_675 ?
C39 H39 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
N3 Os1 N2 96.46(14) . . ?
N3 Os1 N1 98.83(13) . . ?
N2 Os1 N1 79.02(14) . . ?
N3 Os1 O1 87.54(13) . . ?
N2 Os1 O1 172.85(11) . . ?
N1 Os1 O1 94.54(13) . . ?
N3 Os1 O2 174.52(11) . . ?
N2 Os1 O2 86.18(13) . . ?
N1 Os1 O2 86.37(12) . . ?
O1 Os1 O2 90.34(12) . . ?
N3 Os1 N4 78.91(13) . . ?
N2 Os1 N4 101.42(13) . . ?
N1 Os1 N4 177.72(12) . . ?
O1 Os1 N4 85.13(12) . . ?
O2 Os1 N4 95.88(12) . . ?
O5 Cl1 O3 111.5(2) . . ?
O5 Cl1 O4 110.2(3) . . ?
O3 Cl1 O4 108.8(2) . . ?
O5 Cl1 O6 110.1(2) . . ?
O3 Cl1 O6 109.0(3) . . ?
O4 Cl1 O6 107.1(3) . . ?
C11 O2 Os1 126.8(3) . . ?
C1 O1 Os1 127.1(3) . . ?
C33 N4 C29 118.6(3) . . ?
C33 N4 Os1 126.2(3) . . ?
C29 N4 Os1 114.8(3) . . ?
C24 N3 C28 117.6(3) . . ?
C24 N3 Os1 126.5(3) . . ?
C28 N3 Os1 115.8(3) . . ?
C23 N2 C19 117.5(4) . . ?
C23 N2 Os1 125.9(3) . . ?
C19 N2 Os1 116.4(3) . . ?
C14 N1 C18 118.2(3) . . ?
C14 N1 Os1 126.0(3) . . ?
C18 N1 Os1 115.8(3) . . ?
N4 C33 C32 122.0(4) . . ?
N4 C33 H33 119.0 . . ?
C32 C33 H33 119.0 . . ?
C33 C32 C31 119.9(4) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C32 C31 C30 118.5(4) . . ?
C32 C31 H31 120.7 . . ?
C30 C31 H31 120.7 . . ?
C31 C30 C29 120.0(4) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
N4 C29 C30 120.8(4) . . ?
N4 C29 C28 114.1(3) . . ?
C30 C29 C28 125.0(4) . . ?
N3 C28 C27 121.3(4) . . ?
N3 C28 C29 114.1(3) . . ?
C27 C28 C29 124.5(4) . . ?
C26 C27 C28 119.4(4) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C27 C26 C25 119.7(4) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C24 C25 C26 119.0(4) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C25 C24 N3 122.9(4) . . ?
C25 C24 H24 118.5 . . ?
N3 C24 H24 118.5 . . ?
N2 C23 C22 123.3(4) . . ?
N2 C23 H23 118.4 . . ?
C22 C23 H23 118.4 . . ?
C23 C22 C21 119.6(4) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C20 C21 C22 117.9(4) . . ?
C20 C21 H21 121.0 . . ?
C22 C21 H21 121.0 . . ?
C21 C20 C19 120.6(4) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
N2 C19 C20 121.0(4) . . ?
N2 C19 C18 114.3(4) . . ?
C20 C19 C18 124.7(4) . . ?
N1 C18 C17 121.1(4) . . ?
N1 C18 C19 113.9(3) . . ?
C17 C18 C19 124.9(4) . . ?
C16 C17 C18 119.7(4) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C17 C16 C15 119.0(4) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C14 C15 C16 119.5(4) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
N1 C14 C15 122.5(4) . . ?
N1 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C9 C10 C11 121.3(4) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C9 C8 122.8(4) . . ?
C10 C9 H9 118.6 . . ?
C8 C9 H9 118.6 . . ?
C7 C8 C9 122.6(4) . . ?
C7 C8 C13 120.0(4) . . ?
C9 C8 C13 117.3(4) . . ?
C6 C7 C8 121.7(5) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C7 C6 C5 119.3(5) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C5 C4 121.4(5) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C4 C13 119.9(4) . . ?
C5 C4 C3 121.2(5) . . ?
C13 C4 C3 118.9(4) . . ?
C2 C3 C4 121.9(4) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C3 C2 C1 121.2(4) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
O1 C1 C2 115.3(4) . . ?
O1 C1 C12 125.8(4) . . ?
C2 C1 C12 118.9(4) . . ?
C13 C12 C11 119.1(4) . . ?
C13 C12 C1 118.0(4) . . ?
C11 C12 C1 122.9(4) . . ?
O2 C11 C12 126.8(4) . . ?
O2 C11 C10 115.0(4) . . ?
C12 C11 C10 118.3(4) . . ?
C4 C13 C8 117.6(4) . . ?
C4 C13 C12 121.1(4) . . ?
C8 C13 C12 121.3(4) . . ?
C36 C34 C35 118.3(5) 2_665 . ?
C36 C34 H34 120.8 2_665 . ?
C35 C34 H34 120.8 . . ?
C34 C35 C36 121.1(5) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C34 C36 C35 120.6(5) 2_665 . ?
C34 C36 H36 119.7 2_665 . ?
C35 C36 H36 119.7 . . ?
C38 C37 C39 119.9(5) . 2_675 ?
C38 C37 H37 120.0 . . ?
C39 C37 H37 120.0 2_675 . ?
C39 C38 C37 121.4(5) . . ?
C39 C38 H38 119.3 . . ?
C37 C38 H38 119.3 . . ?
C38 C39 C37 118.7(5) . 2_675 ?
C38 C39 H39 120.7 . . ?
C37 C39 H39 120.7 2_675 . ?

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
N3 Os1 O2 C11 -72.0(13) . . . . ?
N2 Os1 O2 C11 169.0(3) . . . . ?
N1 Os1 O2 C11 89.8(3) . . . . ?
O1 Os1 O2 C11 -4.8(3) . . . . ?
N4 Os1 O2 C11 -89.9(3) . . . . ?
N3 Os1 O1 C1 177.4(3) . . . . ?
N2 Os1 O1 C1 -58.3(10) . . . . ?
N1 Os1 O1 C1 -83.9(3) . . . . ?
O2 Os1 O1 C1 2.5(3) . . . . ?
N4 Os1 O1 C1 98.3(3) . . . . ?
N3 Os1 N4 C33 173.3(4) . . . . ?
N2 Os1 N4 C33 78.9(4) . . . . ?
N1 Os1 N4 C33 180(100) . . . . ?
O1 Os1 N4 C33 -98.2(4) . . . . ?
O2 Os1 N4 C33 -8.4(4) . . . . ?
N3 Os1 N4 C29 -13.4(3) . . . . ?
N2 Os1 N4 C29 -107.8(3) . . . . ?
N1 Os1 N4 C29 -7(3) . . . . ?
O1 Os1 N4 C29 75.1(3) . . . . ?
O2 Os1 N4 C29 164.9(3) . . . . ?
N2 Os1 N3 C24 -70.2(4) . . . . ?
N1 Os1 N3 C24 9.6(4) . . . . ?
O1 Os1 N3 C24 103.9(4) . . . . ?
O2 Os1 N3 C24 171.2(11) . . . . ?
N4 Os1 N3 C24 -170.6(4) . . . . ?
N2 Os1 N3 C28 112.6(3) . . . . ?
N1 Os1 N3 C28 -167.5(3) . . . . ?
O1 Os1 N3 C28 -73.3(3) . . . . ?
O2 Os1 N3 C28 -6.0(14) . . . . ?
N4 Os1 N3 C28 12.2(3) . . . . ?
N3 Os1 N2 C23 -80.6(3) . . . . ?
N1 Os1 N2 C23 -178.3(3) . . . . ?
O1 Os1 N2 C23 155.6(8) . . . . ?
O2 Os1 N2 C23 94.6(3) . . . . ?
N4 Os1 N2 C23 -0.6(3) . . . . ?
N3 Os1 N2 C19 104.2(3) . . . . ?
N1 Os1 N2 C19 6.5(3) . . . . ?
O1 Os1 N2 C19 -19.6(11) . . . . ?
O2 Os1 N2 C19 -80.6(3) . . . . ?
N4 Os1 N2 C19 -175.8(3) . . . . ?
N3 Os1 N1 C14 81.5(3) . . . . ?
N2 Os1 N1 C14 176.4(4) . . . . ?
O1 Os1 N1 C14 -6.8(3) . . . . ?
O2 Os1 N1 C14 -96.8(3) . . . . ?
N4 Os1 N1 C14 75(3) . . . . ?
N3 Os1 N1 C18 -102.1(3) . . . . ?
N2 Os1 N1 C18 -7.1(3) . . . . ?
O1 Os1 N1 C18 169.7(3) . . . . ?
O2 Os1 N1 C18 79.7(3) . . . . ?
N4 Os1 N1 C18 -109(3) . . . . ?
C29 N4 C33 C32 -3.9(7) . . . . ?
Os1 N4 C33 C32 169.1(3) . . . . ?
N4 C33 C32 C31 1.0(7) . . . . ?
C33 C32 C31 C30 1.7(7) . . . . ?
C32 C31 C30 C29 -1.4(7) . . . . ?
C33 N4 C29 C30 4.1(6) . . . . ?
Os1 N4 C29 C30 -169.7(3) . . . . ?
C33 N4 C29 C28 -173.8(4) . . . . ?
Os1 N4 C29 C28 12.3(5) . . . . ?
C31 C30 C29 N4 -1.5(7) . . . . ?
C31 C30 C29 C28 176.3(4) . . . . ?
C24 N3 C28 C27 -2.6(6) . . . . ?
Os1 N3 C28 C27 174.8(3) . . . . ?
C24 N3 C28 C29 173.3(4) . . . . ?
Os1 N3 C28 C29 -9.3(5) . . . . ?
N4 C29 C28 N3 -2.2(5) . . . . ?
C30 C29 C28 N3 179.9(4) . . . . ?
N4 C29 C28 C27 173.6(4) . . . . ?
C30 C29 C28 C27 -4.3(7) . . . . ?
N3 C28 C27 C26 1.4(6) . . . . ?
C29 C28 C27 C26 -174.0(4) . . . . ?
C28 C27 C26 C25 0.5(7) . . . . ?
C27 C26 C25 C24 -1.2(7) . . . . ?
C26 C25 C24 N3 -0.1(7) . . . . ?
C28 N3 C24 C25 1.9(6) . . . . ?
Os1 N3 C24 C25 -175.2(3) . . . . ?
C19 N2 C23 C22 1.1(6) . . . . ?
Os1 N2 C23 C22 -174.0(3) . . . . ?
N2 C23 C22 C21 -0.8(7) . . . . ?
C23 C22 C21 C20 0.4(7) . . . . ?
C22 C21 C20 C19 -0.4(7) . . . . ?
C23 N2 C19 C20 -1.1(6) . . . . ?
Os1 N2 C19 C20 174.5(3) . . . . ?
C23 N2 C19 C18 179.5(3) . . . . ?
Os1 N2 C19 C18 -4.8(4) . . . . ?
C21 C20 C19 N2 0.8(7) . . . . ?
C21 C20 C19 C18 -179.9(4) . . . . ?
C14 N1 C18 C17 1.5(6) . . . . ?
Os1 N1 C18 C17 -175.3(3) . . . . ?
C14 N1 C18 C19 -176.6(3) . . . . ?
Os1 N1 C18 C19 6.6(4) . . . . ?
N2 C19 C18 N1 -1.2(5) . . . . ?
C20 C19 C18 N1 179.4(4) . . . . ?
N2 C19 C18 C17 -179.2(4) . . . . ?
C20 C19 C18 C17 1.4(7) . . . . ?
N1 C18 C17 C16 0.1(6) . . . . ?
C19 C18 C17 C16 178.0(4) . . . . ?
C18 C17 C16 C15 -1.7(7) . . . . ?
C17 C16 C15 C14 1.7(7) . . . . ?
C18 N1 C14 C15 -1.5(6) . . . . ?
Os1 N1 C14 C15 174.9(3) . . . . ?
C16 C15 C14 N1 -0.1(7) . . . . ?
C11 C10 C9 C8 1.5(6) . . . . ?
C10 C9 C8 C7 -178.3(4) . . . . ?
C10 C9 C8 C13 -1.7(6) . . . . ?
C9 C8 C7 C6 179.1(4) . . . . ?
C13 C8 C7 C6 2.7(7) . . . . ?
C8 C7 C6 C5 -0.4(7) . . . . ?
C7 C6 C5 C4 -2.1(7) . . . . ?
C6 C5 C4 C13 2.2(7) . . . . ?
C6 C5 C4 C3 -178.5(4) . . . . ?
C5 C4 C3 C2 178.5(4) . . . . ?
C13 C4 C3 C2 -2.2(6) . . . . ?
C4 C3 C2 C1 1.6(7) . . . . ?
Os1 O1 C1 C2 178.8(3) . . . . ?
Os1 O1 C1 C12 0.2(6) . . . . ?
C3 C2 C1 O1 -178.4(4) . . . . ?
C3 C2 C1 C12 0.4(6) . . . . ?
O1 C1 C12 C13 176.9(4) . . . . ?
C2 C1 C12 C13 -1.8(5) . . . . ?
O1 C1 C12 C11 -2.0(6) . . . . ?
C2 C1 C12 C11 179.4(4) . . . . ?
Os1 O2 C11 C12 4.7(6) . . . . ?
Os1 O2 C11 C10 -174.6(2) . . . . ?
C13 C12 C11 O2 -179.5(4) . . . . ?
C1 C12 C11 O2 -0.7(6) . . . . ?
C13 C12 C11 C10 -0.3(6) . . . . ?
C1 C12 C11 C10 178.6(3) . . . . ?
C9 C10 C11 O2 178.9(4) . . . . ?
C9 C10 C11 C12 -0.4(6) . . . . ?
C5 C4 C13 C8 0.1(6) . . . . ?
C3 C4 C13 C8 -179.1(4) . . . . ?
C5 C4 C13 C12 180.0(4) . . . . ?
C3 C4 C13 C12 0.7(6) . . . . ?
C7 C8 C13 C4 -2.5(6) . . . . ?
C9 C8 C13 C4 -179.1(4) . . . . ?
C7 C8 C13 C12 177.6(4) . . . . ?
C9 C8 C13 C12 1.0(6) . . . . ?
C11 C12 C13 C4 -179.9(4) . . . . ?
C1 C12 C13 C4 1.2(6) . . . . ?
C11 C12 C13 C8 0.0(6) . . . . ?
C1 C12 C13 C8 -178.9(4) . . . . ?
C36 C34 C35 C36 0.6(9) 2_665 . . . ?
C34 C35 C36 C34 -0.7(9) . . . 2_665 ?
C39 C37 C38 C39 0.8(8) 2_675 . . . ?
C37 C38 C39 C37 -0.8(8) . . . 2_675 ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_2ClO4
_database_code_depnum_ccdc_archive 'CCDC 1465138'
_audit_update_record             
;
2016-03-12 deposited with the CCDC.
2016-10-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H25 Cl N6 O6 Os'
_chemical_formula_weight         851.26

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'

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

_cell_length_a                   10.552(2)
_cell_length_b                   19.785(3)
_cell_length_c                   15.902(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.0190(10)
_cell_angle_gamma                90.00
_cell_volume                     3138.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6139
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      29.2

_exptl_crystal_description       Prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1672
_exptl_absorpt_coefficient_mu    4.207
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2907
_exptl_absorpt_correction_T_max  0.8842
_exptl_absorpt_process_details   
'(a) Busing, W. R.; Levy, H. A. Acta Crystallogr. 1957, 10, 180-182. (b) Coppens, P.; Leiserowitz, L.; Rabinovich, D. Acta Crystallogr. 1965, 18, 1035-1038'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22375
_diffrn_reflns_av_R_equivalents  0.1005
_diffrn_reflns_av_sigmaI/netI    0.0881
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.37
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5441
_reflns_number_gt                4489
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  ORTEP

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0435P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5441
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1115
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.87798(2) 0.147299(12) 0.714195(15) 0.01864(12) Uani 1 1 d . . .
Cl2 Cl 0.43161(17) -0.04653(9) 0.76817(11) 0.0291(4) Uani 1 1 d . . .
O2 O 1.0165(4) 0.0857(2) 0.7970(3) 0.0211(10) Uani 1 1 d . . .
O1 O 0.7717(4) 0.13867(19) 0.7996(3) 0.0196(10) Uani 1 1 d . . .
O5 O 0.5070(5) -0.1092(2) 0.7845(3) 0.0392(12) Uani 1 1 d . . .
O3 O 0.5221(5) 0.0098(2) 0.7914(3) 0.0409(13) Uani 1 1 d . . .
O6 O 0.3549(5) -0.0433(3) 0.6745(3) 0.0497(15) Uani 1 1 d . . .
O4 O 0.3455(6) -0.0449(3) 0.8196(4) 0.0655(18) Uani 1 1 d . . .
N3 N 0.9846(6) 0.1327(2) 0.6356(3) 0.0195(12) Uani 1 1 d . . .
N2 N 0.9650(5) 0.0778(2) 0.5842(3) 0.0234(12) Uani 1 1 d . . .
N1 N 0.7866(5) 0.0669(2) 0.6407(3) 0.0197(12) Uani 1 1 d . . .
N4 N 0.7516(5) 0.2207(3) 0.6587(3) 0.0214(12) Uani 1 1 d . . .
N5 N 0.7489(5) 0.2728(3) 0.7092(3) 0.0224(12) Uani 1 1 d . . .
N6 N 0.9619(5) 0.2290(2) 0.7894(3) 0.0177(11) Uani 1 1 d . . .
C11 C 1.0443(7) 0.0830(3) 0.8834(4) 0.0225(15) Uani 1 1 d . . .
C10 C 1.1753(6) 0.0597(3) 0.9318(4) 0.0240(15) Uani 1 1 d . . .
H10 H 1.2354 0.0472 0.9011 0.029 Uiso 1 1 calc R . .
C9 C 1.2145(6) 0.0555(3) 1.0220(4) 0.0239(15) Uani 1 1 d . . .
H9 H 1.3039 0.0422 1.0537 0.029 Uiso 1 1 calc R . .
C8 C 1.1260(6) 0.0704(3) 1.0703(4) 0.0214(15) Uani 1 1 d . . .
C13 C 0.9943(6) 0.0913(3) 1.0234(4) 0.0193(14) Uani 1 1 d . . .
C12 C 0.9523(6) 0.1006(3) 0.9281(4) 0.0187(14) Uani 1 1 d . . .
C1 C 0.8180(6) 0.1236(3) 0.8840(4) 0.0216(14) Uani 1 1 d . . .
C2 C 0.7260(7) 0.1286(3) 0.9324(4) 0.0242(15) Uani 1 1 d . . .
H2 H 0.6345 0.1384 0.9013 0.029 Uiso 1 1 calc R . .
C3 C 0.7661(7) 0.1196(3) 1.0219(4) 0.0253(15) Uani 1 1 d . . .
H3 H 0.7039 0.1255 1.0531 0.030 Uiso 1 1 calc R . .
C4 C 0.9021(6) 0.1011(3) 1.0694(4) 0.0227(15) Uani 1 1 d . . .
C5 C 0.9445(7) 0.0930(3) 1.1623(4) 0.0276(16) Uani 1 1 d . . .
H5 H 0.8828 0.1003 1.1936 0.033 Uiso 1 1 calc R . .
C6 C 1.0751(7) 0.0744(3) 1.2086(4) 0.0289(16) Uani 1 1 d . . .
H6 H 1.1029 0.0706 1.2716 0.035 Uiso 1 1 calc R . .
C7 C 1.1653(7) 0.0614(3) 1.1645(4) 0.0259(16) Uani 1 1 d . . .
H7 H 1.2534 0.0464 1.1966 0.031 Uiso 1 1 calc R . .
C19 C 1.2277(7) 0.1217(4) 0.6715(4) 0.0288(16) Uani 1 1 d . . .
H19 H 1.2193 0.0740 0.6738 0.035 Uiso 1 1 calc R . .
C20 C 1.3511(8) 0.1508(3) 0.6904(5) 0.0327(19) Uani 1 1 d . . .
H20 H 1.4287 0.1230 0.7066 0.039 Uiso 1 1 calc R . .
C21 C 1.3655(7) 0.2199(4) 0.6866(4) 0.0318(17) Uani 1 1 d . . .
H21 H 1.4523 0.2393 0.7007 0.038 Uiso 1 1 calc R . .
C22 C 1.2534(8) 0.2608(4) 0.6622(4) 0.0357(18) Uani 1 1 d . . .
H22 H 1.2633 0.3083 0.6577 0.043 Uiso 1 1 calc R . .
C23 C 1.1278(7) 0.2335(3) 0.6444(4) 0.0279(16) Uani 1 1 d . . .
H23 H 1.0510 0.2619 0.6294 0.034 Uiso 1 1 calc R . .
C24 C 1.1140(7) 0.1627(3) 0.6486(4) 0.0225(15) Uani 1 1 d . . .
C18 C 0.8519(6) 0.0444(3) 0.5835(4) 0.0206(14) Uani 1 1 d . . .
C17 C 0.8044(6) -0.0106(3) 0.5278(4) 0.0230(15) Uani 1 1 d . . .
H17 H 0.8496 -0.0250 0.4881 0.028 Uiso 1 1 calc R . .
C16 C 0.6919(6) -0.0437(3) 0.5305(4) 0.0251(16) Uani 1 1 d . . .
H16 H 0.6578 -0.0813 0.4926 0.030 Uiso 1 1 calc R . .
C15 C 0.6279(7) -0.0217(3) 0.5898(4) 0.0289(16) Uani 1 1 d . . .
H15 H 0.5516 -0.0451 0.5941 0.035 Uiso 1 1 calc R . .
C14 C 0.6760(6) 0.0342(3) 0.6419(4) 0.0215(14) Uani 1 1 d . . .
H14 H 0.6294 0.0501 0.6801 0.026 Uiso 1 1 calc R . .
C25 C 0.6580(7) 0.1852(3) 0.5037(4) 0.0299(17) Uani 1 1 d . . .
H25 H 0.7316 0.1553 0.5126 0.036 Uiso 1 1 calc R . .
C26 C 0.5586(7) 0.1900(3) 0.4210(4) 0.0342(17) Uani 1 1 d . . .
H26 H 0.5649 0.1633 0.3728 0.041 Uiso 1 1 calc R . .
C27 C 0.4514(7) 0.2329(3) 0.4083(4) 0.0316(17) Uani 1 1 d . . .
H27 H 0.3815 0.2339 0.3526 0.038 Uiso 1 1 calc R . .
C28 C 0.4454(7) 0.2748(3) 0.4770(4) 0.0298(16) Uani 1 1 d . . .
H28 H 0.3741 0.3063 0.4669 0.036 Uiso 1 1 calc R . .
C29 C 0.5428(6) 0.2711(3) 0.5602(4) 0.0233(15) Uani 1 1 d . . .
H29 H 0.5383 0.2992 0.6076 0.028 Uiso 1 1 calc R . .
C30 C 0.6473(6) 0.2251(3) 0.5727(4) 0.0213(14) Uani 1 1 d . . .
C31 C 0.8622(6) 0.2762(3) 0.7833(4) 0.0202(14) Uani 1 1 d . . .
C32 C 0.8824(7) 0.3307(3) 0.8437(4) 0.0266(16) Uani 1 1 d . . .
H32 H 0.8133 0.3626 0.8393 0.032 Uiso 1 1 calc R . .
C33 C 1.0038(7) 0.3359(3) 0.9083(4) 0.0278(17) Uani 1 1 d . . .
H33 H 1.0183 0.3704 0.9519 0.033 Uiso 1 1 calc R . .
C34 C 1.1071(6) 0.2912(3) 0.9112(4) 0.0251(15) Uani 1 1 d . . .
H34 H 1.1938 0.2972 0.9535 0.030 Uiso 1 1 calc R . .
C35 C 1.0816(6) 0.2383(3) 0.8516(4) 0.0229(15) Uani 1 1 d . . .
H35 H 1.1516 0.2072 0.8549 0.028 Uiso 1 1 calc R . .


_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 N3 1.956(6) . ?
Os1 N4 1.974(5) . ?
Os1 N1 2.022(5) . ?
Os1 O2 2.026(4) . ?
Os1 O1 2.030(4) . ?
Os1 N6 2.035(5) . ?
Cl2 O4 1.408(5) . ?
Cl2 O3 1.435(5) . ?
Cl2 O6 1.447(5) . ?
Cl2 O5 1.450(5) . ?
O2 C11 1.308(7) . ?
O1 C1 1.305(7) . ?
N3 N2 1.335(7) . ?
N3 C24 1.440(8) . ?
N2 C18 1.361(8) . ?
N1 C14 1.341(8) . ?
N1 C18 1.380(8) . ?
N4 N5 1.312(6) . ?
N4 C30 1.452(7) . ?
N5 C31 1.380(8) . ?
N6 C35 1.339(8) . ?
N6 C31 1.385(8) . ?
C11 C12 1.421(8) . ?
C11 C10 1.422(9) . ?
C10 C9 1.361(8) . ?
C10 H10 0.9500 . ?
C9 C8 1.420(9) . ?
C9 H9 0.9500 . ?
C8 C13 1.408(8) . ?
C8 C7 1.429(8) . ?
C13 C4 1.408(8) . ?
C13 C12 1.446(8) . ?
C12 C1 1.435(8) . ?
C1 C2 1.425(9) . ?
C2 C3 1.357(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.434(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.408(8) . ?
C5 C6 1.384(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.379(9) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C19 C20 1.365(9) . ?
C19 C24 1.395(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.378(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.380(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.373(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.411(8) . ?
C23 H23 0.9500 . ?
C18 C17 1.389(8) . ?
C17 C16 1.370(9) . ?
C17 H17 0.9500 . ?
C16 C15 1.397(9) . ?
C16 H16 0.9500 . ?
C15 C14 1.376(8) . ?
C15 H15 0.9500 . ?
C14 H14 0.9500 . ?
C25 C30 1.386(8) . ?
C25 C26 1.393(9) . ?
C25 H25 0.9500 . ?
C26 C27 1.376(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.389(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.388(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.393(8) . ?
C29 H29 0.9500 . ?
C31 C32 1.413(8) . ?
C32 C33 1.360(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.392(9) . ?
C33 H33 0.9500 . ?
C34 C35 1.378(8) . ?
C34 H34 0.9500 . ?
C35 H35 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
N3 Os1 N4 105.5(2) . . ?
N3 Os1 N1 77.3(2) . . ?
N4 Os1 N1 101.2(2) . . ?
N3 Os1 O2 83.31(18) . . ?
N4 Os1 O2 166.50(18) . . ?
N1 Os1 O2 90.58(18) . . ?
N3 Os1 O1 166.60(19) . . ?
N4 Os1 O1 85.47(19) . . ?
N1 Os1 O1 93.30(19) . . ?
O2 Os1 O1 87.32(16) . . ?
N3 Os1 N6 105.2(2) . . ?
N4 Os1 N6 77.3(2) . . ?
N1 Os1 N6 177.36(19) . . ?
O2 Os1 N6 90.70(18) . . ?
O1 Os1 N6 84.45(18) . . ?
O4 Cl2 O3 109.5(3) . . ?
O4 Cl2 O6 110.3(4) . . ?
O3 Cl2 O6 109.5(3) . . ?
O4 Cl2 O5 109.6(3) . . ?
O3 Cl2 O5 109.8(3) . . ?
O6 Cl2 O5 108.2(3) . . ?
C11 O2 Os1 125.1(4) . . ?
C1 O1 Os1 127.2(4) . . ?
N2 N3 C24 112.0(5) . . ?
N2 N3 Os1 120.3(4) . . ?
C24 N3 Os1 124.3(4) . . ?
N3 N2 C18 111.2(5) . . ?
C14 N1 C18 118.5(5) . . ?
C14 N1 Os1 128.6(4) . . ?
C18 N1 Os1 112.9(4) . . ?
N5 N4 C30 111.6(5) . . ?
N5 N4 Os1 116.7(4) . . ?
C30 N4 Os1 131.3(4) . . ?
N4 N5 C31 112.0(5) . . ?
C35 N6 C31 118.1(5) . . ?
C35 N6 Os1 131.9(4) . . ?
C31 N6 Os1 108.6(4) . . ?
O2 C11 C12 124.0(6) . . ?
O2 C11 C10 115.3(6) . . ?
C12 C11 C10 120.7(5) . . ?
C9 C10 C11 119.9(6) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C9 C8 122.0(6) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C13 C8 C9 119.0(5) . . ?
C13 C8 C7 119.4(6) . . ?
C9 C8 C7 121.6(6) . . ?
C4 C13 C8 119.7(5) . . ?
C4 C13 C12 119.9(5) . . ?
C8 C13 C12 120.3(5) . . ?
C11 C12 C1 124.1(5) . . ?
C11 C12 C13 117.9(5) . . ?
C1 C12 C13 118.0(5) . . ?
O1 C1 C2 116.6(6) . . ?
O1 C1 C12 123.6(6) . . ?
C2 C1 C12 119.8(5) . . ?
C3 C2 C1 121.5(6) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 120.1(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C13 119.5(6) . . ?
C5 C4 C3 120.2(6) . . ?
C13 C4 C3 120.3(5) . . ?
C6 C5 C4 120.6(6) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C7 C6 C5 120.8(6) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C8 119.8(6) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C20 C19 C24 119.3(7) . . ?
C20 C19 H19 120.4 . . ?
C24 C19 H19 120.4 . . ?
C19 C20 C21 121.3(7) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C22 119.8(7) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C23 C22 C21 120.6(7) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C24 119.2(6) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C19 C24 C23 119.8(6) . . ?
C19 C24 N3 119.5(6) . . ?
C23 C24 N3 120.6(6) . . ?
N2 C18 N1 117.5(6) . . ?
N2 C18 C17 121.2(6) . . ?
N1 C18 C17 121.3(6) . . ?
C16 C17 C18 119.4(6) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C16 C15 119.1(6) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C14 C15 C16 119.5(6) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
N1 C14 C15 122.1(6) . . ?
N1 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C30 C25 C26 118.6(6) . . ?
C30 C25 H25 120.7 . . ?
C26 C25 H25 120.7 . . ?
C27 C26 C25 120.7(7) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C28 119.9(6) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 120.6(6) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C30 118.4(6) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C25 C30 C29 121.6(6) . . ?
C25 C30 N4 118.6(6) . . ?
C29 C30 N4 119.7(6) . . ?
N5 C31 N6 117.0(5) . . ?
N5 C31 C32 120.9(6) . . ?
N6 C31 C32 121.6(6) . . ?
C33 C32 C31 117.9(6) . . ?
C33 C32 H32 121.1 . . ?
C31 C32 H32 121.1 . . ?
C32 C33 C34 120.7(6) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C35 C34 C33 119.0(6) . . ?
C35 C34 H34 120.5 . . ?
C33 C34 H34 120.5 . . ?
N6 C35 C34 122.5(6) . . ?
N6 C35 H35 118.7 . . ?
C34 C35 H35 118.7 . . ?

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
N3 Os1 O2 C11 157.8(5) . . . . ?
N4 Os1 O2 C11 25.9(11) . . . . ?
N1 Os1 O2 C11 -125.1(5) . . . . ?
O1 Os1 O2 C11 -31.8(5) . . . . ?
N6 Os1 O2 C11 52.6(5) . . . . ?
N3 Os1 O1 C1 69.6(9) . . . . ?
N4 Os1 O1 C1 -144.6(5) . . . . ?
N1 Os1 O1 C1 114.4(5) . . . . ?
O2 Os1 O1 C1 24.0(5) . . . . ?
N6 Os1 O1 C1 -67.0(5) . . . . ?
N4 Os1 N3 N2 -106.9(4) . . . . ?
N1 Os1 N3 N2 -8.7(4) . . . . ?
O2 Os1 N3 N2 83.4(4) . . . . ?
O1 Os1 N3 N2 37.5(10) . . . . ?
N6 Os1 N3 N2 172.4(4) . . . . ?
N4 Os1 N3 C24 95.8(5) . . . . ?
N1 Os1 N3 C24 -165.9(5) . . . . ?
O2 Os1 N3 C24 -73.8(5) . . . . ?
O1 Os1 N3 C24 -119.7(8) . . . . ?
N6 Os1 N3 C24 15.1(5) . . . . ?
C24 N3 N2 C18 170.8(5) . . . . ?
Os1 N3 N2 C18 11.0(6) . . . . ?
N3 Os1 N1 C14 -176.6(5) . . . . ?
N4 Os1 N1 C14 -73.0(5) . . . . ?
O2 Os1 N1 C14 100.4(5) . . . . ?
O1 Os1 N1 C14 13.0(5) . . . . ?
N6 Os1 N1 C14 -19(4) . . . . ?
N3 Os1 N1 C18 4.2(4) . . . . ?
N4 Os1 N1 C18 107.8(4) . . . . ?
O2 Os1 N1 C18 -78.8(4) . . . . ?
O1 Os1 N1 C18 -166.1(4) . . . . ?
N6 Os1 N1 C18 162(4) . . . . ?
N3 Os1 N4 N5 -126.9(4) . . . . ?
N1 Os1 N4 N5 153.3(4) . . . . ?
O2 Os1 N4 N5 2.9(11) . . . . ?
O1 Os1 N4 N5 60.8(4) . . . . ?
N6 Os1 N4 N5 -24.5(4) . . . . ?
N3 Os1 N4 C30 60.9(6) . . . . ?
N1 Os1 N4 C30 -18.9(6) . . . . ?
O2 Os1 N4 C30 -169.3(6) . . . . ?
O1 Os1 N4 C30 -111.3(5) . . . . ?
N6 Os1 N4 C30 163.3(6) . . . . ?
C30 N4 N5 C31 -168.0(5) . . . . ?
Os1 N4 N5 C31 18.3(6) . . . . ?
N3 Os1 N6 C35 -66.8(6) . . . . ?
N4 Os1 N6 C35 -169.7(6) . . . . ?
N1 Os1 N6 C35 135(4) . . . . ?
O2 Os1 N6 C35 16.4(6) . . . . ?
O1 Os1 N6 C35 103.7(6) . . . . ?
N3 Os1 N6 C31 127.2(4) . . . . ?
N4 Os1 N6 C31 24.3(4) . . . . ?
N1 Os1 N6 C31 -31(4) . . . . ?
O2 Os1 N6 C31 -149.6(4) . . . . ?
O1 Os1 N6 C31 -62.3(4) . . . . ?
Os1 O2 C11 C12 26.1(8) . . . . ?
Os1 O2 C11 C10 -154.8(4) . . . . ?
O2 C11 C10 C9 179.5(6) . . . . ?
C12 C11 C10 C9 -1.3(9) . . . . ?
C11 C10 C9 C8 3.3(10) . . . . ?
C10 C9 C8 C13 -1.1(9) . . . . ?
C10 C9 C8 C7 175.6(6) . . . . ?
C9 C8 C13 C4 175.0(6) . . . . ?
C7 C8 C13 C4 -1.9(9) . . . . ?
C9 C8 C13 C12 -3.0(9) . . . . ?
C7 C8 C13 C12 -179.8(6) . . . . ?
O2 C11 C12 C1 -0.1(10) . . . . ?
C10 C11 C12 C1 -179.2(6) . . . . ?
O2 C11 C12 C13 176.5(5) . . . . ?
C10 C11 C12 C13 -2.6(9) . . . . ?
C4 C13 C12 C11 -173.2(6) . . . . ?
C8 C13 C12 C11 4.7(9) . . . . ?
C4 C13 C12 C1 3.6(9) . . . . ?
C8 C13 C12 C1 -178.4(6) . . . . ?
Os1 O1 C1 C2 172.7(4) . . . . ?
Os1 O1 C1 C12 -9.7(9) . . . . ?
C11 C12 C1 O1 -8.7(10) . . . . ?
C13 C12 C1 O1 174.7(6) . . . . ?
C11 C12 C1 C2 168.9(6) . . . . ?
C13 C12 C1 C2 -7.7(9) . . . . ?
O1 C1 C2 C3 -174.5(6) . . . . ?
C12 C1 C2 C3 7.8(10) . . . . ?
C1 C2 C3 C4 -3.3(10) . . . . ?
C8 C13 C4 C5 3.0(9) . . . . ?
C12 C13 C4 C5 -179.0(6) . . . . ?
C8 C13 C4 C3 -177.3(6) . . . . ?
C12 C13 C4 C3 0.7(9) . . . . ?
C2 C3 C4 C5 178.8(6) . . . . ?
C2 C3 C4 C13 -0.9(10) . . . . ?
C13 C4 C5 C6 -1.1(10) . . . . ?
C3 C4 C5 C6 179.2(6) . . . . ?
C4 C5 C6 C7 -2.1(10) . . . . ?
C5 C6 C7 C8 3.2(10) . . . . ?
C13 C8 C7 C6 -1.2(9) . . . . ?
C9 C8 C7 C6 -178.0(6) . . . . ?
C24 C19 C20 C21 -0.7(10) . . . . ?
C19 C20 C21 C22 -0.7(11) . . . . ?
C20 C21 C22 C23 2.0(10) . . . . ?
C21 C22 C23 C24 -1.9(9) . . . . ?
C20 C19 C24 C23 0.8(9) . . . . ?
C20 C19 C24 N3 -175.0(6) . . . . ?
C22 C23 C24 C19 0.5(9) . . . . ?
C22 C23 C24 N3 176.2(6) . . . . ?
N2 N3 C24 C19 -47.0(7) . . . . ?
Os1 N3 C24 C19 111.8(6) . . . . ?
N2 N3 C24 C23 137.2(6) . . . . ?
Os1 N3 C24 C23 -63.9(7) . . . . ?
N3 N2 C18 N1 -6.7(7) . . . . ?
N3 N2 C18 C17 173.6(5) . . . . ?
C14 N1 C18 N2 -179.1(5) . . . . ?
Os1 N1 C18 N2 0.1(7) . . . . ?
C14 N1 C18 C17 0.5(8) . . . . ?
Os1 N1 C18 C17 179.8(4) . . . . ?
N2 C18 C17 C16 178.6(5) . . . . ?
N1 C18 C17 C16 -1.1(9) . . . . ?
C18 C17 C16 C15 -0.4(9) . . . . ?
C17 C16 C15 C14 2.3(9) . . . . ?
C18 N1 C14 C15 1.5(8) . . . . ?
Os1 N1 C14 C15 -177.6(4) . . . . ?
C16 C15 C14 N1 -2.9(9) . . . . ?
C30 C25 C26 C27 -0.6(10) . . . . ?
C25 C26 C27 C28 3.6(10) . . . . ?
C26 C27 C28 C29 -3.8(10) . . . . ?
C27 C28 C29 C30 0.9(10) . . . . ?
C26 C25 C30 C29 -2.3(10) . . . . ?
C26 C25 C30 N4 -179.4(6) . . . . ?
C28 C29 C30 C25 2.2(10) . . . . ?
C28 C29 C30 N4 179.2(6) . . . . ?
N5 N4 C30 C25 162.6(6) . . . . ?
Os1 N4 C30 C25 -24.9(9) . . . . ?
N5 N4 C30 C29 -14.5(8) . . . . ?
Os1 N4 C30 C29 158.0(5) . . . . ?
N4 N5 C31 N6 4.6(8) . . . . ?
N4 N5 C31 C32 176.5(6) . . . . ?
C35 N6 C31 N5 168.4(5) . . . . ?
Os1 N6 C31 N5 -23.4(6) . . . . ?
C35 N6 C31 C32 -3.4(9) . . . . ?
Os1 N6 C31 C32 164.8(5) . . . . ?
N5 C31 C32 C33 -171.1(6) . . . . ?
N6 C31 C32 C33 0.4(10) . . . . ?
C31 C32 C33 C34 3.8(10) . . . . ?
C32 C33 C34 C35 -4.9(10) . . . . ?
C31 N6 C35 C34 2.3(9) . . . . ?
Os1 N6 C35 C34 -162.6(5) . . . . ?
C33 C34 C35 N6 1.8(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         2.678
_refine_diff_density_min         -2.202
_refine_diff_density_rms         0.189
