#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:12:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179317 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/14/4321439.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4321439
loop_
_publ_author_name
'Peter Barthazy'
'Michael Wörle'
'Heinz Rüegger'
'Antonio Mezzetti'
_publ_section_title
;
 Oxo Complexes of Osmium(IV) Formed via Dioxygen Activation. X-ray
 Structures of [OsX(dcpe)2]PF6 (X = Cl, Br), [OsCl(η2-O2)(dcpe)2]BPh4,
 and [OsCl(O)(dcpe)2]BPh4 (dcpe = 1,2-Bis(dicyclohexylphosphino)ethane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4903
_journal_page_last               4912
_journal_paper_doi               10.1021/ic0002420
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C77 H118 B Cl3 O2 Os P4'
_chemical_formula_weight         1506.95
_chemical_name_common            '[OsCl(O2)(dcpe)2]BPh4'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.9880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.585(4)
_cell_length_b                   12.764(2)
_cell_length_c                   25.587(4)
_cell_measurement_temperature    293(2)
_cell_volume                     7474(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART PLATFORM with CCD detector'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_sigmaI/netI    0.0964
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            61602
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    1.943
_exptl_absorpt_correction_type   'empirical (SADABS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.765
_refine_diff_density_min         -1.851
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.973
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         18573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_restrained_S_obs      1.044
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_obs          0.0460
_refine_ls_shift/esd_max         0.014
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0459P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1181
_refine_ls_wR_factor_obs         0.0999
_reflns_number_observed          11786
_reflns_number_total             18573
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0002420_3.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7474.5(19)
_cod_database_code               4321439
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'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Os Os 0.737629(7) 0.760678(12) 0.443230(7) 0.03218(6) Uani 1 d . .
Cl1 Cl 0.71174(5) 0.59952(9) 0.47806(5) 0.0422(3) Uani 1 d . .
P1 P 0.67373(5) 0.67740(8) 0.36105(4) 0.0317(3) Uani 1 d . .
P2 P 0.81457(5) 0.66106(9) 0.41346(5) 0.0351(3) Uani 1 d . .
P3 P 0.78976(6) 0.79708(10) 0.53787(5) 0.0401(3) Uani 1 d . .
P4 P 0.66370(5) 0.86892(9) 0.46871(5) 0.0367(3) Uani 1 d . .
O1 O 0.7429(2) 0.8743(3) 0.39047(15) 0.0532(9) Uani 1 d . .
O2 O 0.7781(2) 0.8998(3) 0.4369(2) 0.0663(11) Uani 1 d . .
C1 C 0.6040(2) 0.6206(3) 0.3707(2) 0.0376(11) Uani 1 d . .
H1A H 0.6054(2) 0.6294(3) 0.4090(2) 0.045 Uiso 1 calc R .
C2 C 0.5977(2) 0.5024(3) 0.3600(2) 0.0482(13) Uani 1 d . .
H2A H 0.5977(2) 0.4886(3) 0.3227(2) 0.058 Uiso 1 calc R .
H2B H 0.6309(2) 0.4663(3) 0.3826(2) 0.058 Uiso 1 calc R .
C3 C 0.5411(2) 0.4604(4) 0.3715(2) 0.062(2) Uani 1 d . .
H3A H 0.5370(2) 0.3869(4) 0.3615(2) 0.075 Uiso 1 calc R .
H3B H 0.5439(2) 0.4652(4) 0.4098(2) 0.075 Uiso 1 calc R .
C4 C 0.4871(2) 0.5189(4) 0.3414(2) 0.067(2) Uani 1 d . .
H4A H 0.4815(2) 0.5080(4) 0.3030(2) 0.081 Uiso 1 calc R .
H4B H 0.4530(2) 0.4918(4) 0.3519(2) 0.081 Uiso 1 calc R .
C5 C 0.4932(2) 0.6347(4) 0.3538(2) 0.0573(14) Uani 1 d . .
H5A H 0.4955(2) 0.6459(4) 0.3917(2) 0.069 Uiso 1 calc R .
H5B H 0.4590(2) 0.6713(4) 0.3332(2) 0.069 Uiso 1 calc R .
C6 C 0.5478(2) 0.6791(4) 0.3399(2) 0.0464(12) Uani 1 d . .
H6A H 0.5512(2) 0.7529(4) 0.3491(2) 0.056 Uiso 1 calc R .
H6B H 0.5440(2) 0.6727(4) 0.3014(2) 0.056 Uiso 1 calc R .
C7 C 0.6524(2) 0.7456(3) 0.2942(2) 0.0379(10) Uani 1 d . .
H7A H 0.6193(2) 0.7904(3) 0.2964(2) 0.045 Uiso 1 calc R .
C8 C 0.6288(2) 0.6713(4) 0.2475(2) 0.0511(13) Uani 1 d . .
H8A H 0.6605(2) 0.6294(4) 0.2407(2) 0.061 Uiso 1 calc R .
H8B H 0.6005(2) 0.6243(4) 0.2569(2) 0.061 Uiso 1 calc R .
C9 C 0.6000(3) 0.7317(4) 0.1971(2) 0.068(2) Uani 1 d . .
H9A H 0.5856(3) 0.6828(4) 0.1679(2) 0.082 Uiso 1 calc R .
H9B H 0.5668(3) 0.7702(4) 0.2034(2) 0.082 Uiso 1 calc R .
C10 C 0.6419(3) 0.8068(5) 0.1812(2) 0.073(2) Uani 1 d . .
H10A H 0.6215(3) 0.8475(5) 0.1504(2) 0.088 Uiso 1 calc R .
H10B H 0.6727(3) 0.7677(5) 0.1708(2) 0.088 Uiso 1 calc R .
C11 C 0.6683(3) 0.8794(5) 0.2269(2) 0.069(2) Uani 1 d . .
H11A H 0.6382(3) 0.9254(5) 0.2338(2) 0.083 Uiso 1 calc R .
H11B H 0.6978(3) 0.9226(5) 0.2167(2) 0.083 Uiso 1 calc R .
C12 C 0.6965(2) 0.8183(5) 0.2787(2) 0.062(2) Uani 1 d . .
H12A H 0.7292(2) 0.7777(5) 0.2730(2) 0.074 Uiso 1 calc R .
H12B H 0.7112(2) 0.8673(5) 0.3078(2) 0.074 Uiso 1 calc R .
C13 C 0.7176(2) 0.5653(3) 0.3483(2) 0.0411(11) Uani 1 d . .
H13A H 0.7187(2) 0.5122(3) 0.3757(2) 0.049 Uiso 1 calc R .
H13B H 0.6996(2) 0.5348(3) 0.3135(2) 0.049 Uiso 1 calc R .
C14 C 0.7788(2) 0.6002(4) 0.3492(2) 0.0406(11) Uani 1 d . .
H14A H 0.7775(2) 0.6499(4) 0.3203(2) 0.049 Uiso 1 calc R .
H14B H 0.8015(2) 0.5401(4) 0.3429(2) 0.049 Uiso 1 calc R .
C15 C 0.8778(2) 0.7246(4) 0.3953(2) 0.0443(12) Uani 1 d . .
H15A H 0.9050(2) 0.7450(4) 0.4292(2) 0.053 Uiso 1 calc R .
C16 C 0.8625(2) 0.8248(4) 0.3618(2) 0.059(2) Uani 1 d . .
H16A H 0.8366(2) 0.8073(4) 0.3273(2) 0.071 Uiso 1 calc R .
H16B H 0.8420(2) 0.8726(4) 0.3802(2) 0.071 Uiso 1 calc R .
C17 C 0.9166(3) 0.8788(5) 0.3524(3) 0.076(2) Uani 1 d . .
H17A H 0.9413(3) 0.9007(5) 0.3867(3) 0.091 Uiso 1 calc R .
H17B H 0.9050(3) 0.9409(5) 0.3306(3) 0.091 Uiso 1 calc R .
C18 C 0.9510(3) 0.8065(5) 0.3242(3) 0.082(2) Uani 1 d . .
H18A H 0.9281(3) 0.7913(5) 0.2881(3) 0.098 Uiso 1 calc R .
H18B H 0.9867(3) 0.8411(5) 0.3212(3) 0.098 Uiso 1 calc R .
C19 C 0.9660(2) 0.7050(5) 0.3553(2) 0.074(2) Uani 1 d . .
H19A H 0.9932(2) 0.7195(5) 0.3895(2) 0.089 Uiso 1 calc R .
H19B H 0.9850(2) 0.6579(5) 0.3351(2) 0.089 Uiso 1 calc R .
C20 C 0.9117(2) 0.6515(4) 0.3656(2) 0.0581(15) Uani 1 d . .
H20A H 0.9234(2) 0.5889(4) 0.3870(2) 0.070 Uiso 1 calc R .
H20B H 0.8863(2) 0.6303(4) 0.3315(2) 0.070 Uiso 1 calc R .
C21 C 0.8463(2) 0.5496(3) 0.4579(2) 0.0386(11) Uani 1 d . .
H21A H 0.8206(2) 0.5409(3) 0.4826(2) 0.046 Uiso 1 calc R .
C22 C 0.8453(2) 0.4430(3) 0.4298(2) 0.0548(15) Uani 1 d . .
H22A H 0.8708(2) 0.4456(3) 0.4052(2) 0.066 Uiso 1 calc R .
H22B H 0.8060(2) 0.4282(3) 0.4090(2) 0.066 Uiso 1 calc R .
C23 C 0.8657(3) 0.3552(4) 0.4714(2) 0.068(2) Uani 1 d . .
H23A H 0.8383(3) 0.3489(4) 0.4941(2) 0.081 Uiso 1 calc R .
H23B H 0.8661(3) 0.2891(4) 0.4528(2) 0.081 Uiso 1 calc R .
C24 C 0.9254(3) 0.3772(4) 0.5058(2) 0.068(2) Uani 1 d . .
H24A H 0.9534(3) 0.3782(4) 0.4835(2) 0.082 Uiso 1 calc R .
H24B H 0.9367(3) 0.3218(4) 0.5322(2) 0.082 Uiso 1 calc R .
C25 C 0.9269(2) 0.4811(4) 0.5343(2) 0.0587(15) Uani 1 d . .
H25A H 0.9664(2) 0.4948(4) 0.5551(2) 0.070 Uiso 1 calc R .
H25B H 0.9017(2) 0.4778(4) 0.5591(2) 0.070 Uiso 1 calc R .
C26 C 0.9070(2) 0.5708(4) 0.4944(2) 0.0438(12) Uani 1 d . .
H26A H 0.9349(2) 0.5794(4) 0.4723(2) 0.053 Uiso 1 calc R .
H26B H 0.9061(2) 0.6354(4) 0.5141(2) 0.053 Uiso 1 calc R .
C27A C 0.8481(4) 0.8997(8) 0.5531(3) 0.051(2) Uiso 0.692(5) d P .
C27B C 0.8421(10) 0.9038(17) 0.5359(8) 0.051(2) Uiso 0.308(5) d P .
C28A C 0.8263(4) 1.0134(6) 0.5442(3) 0.058(2) Uiso 0.692(5) d P .
C28B C 0.8620(8) 0.9681(13) 0.5895(7) 0.058(2) Uiso 0.308(5) d P .
C29A C 0.8757(4) 1.0920(7) 0.5572(4) 0.059(2) Uiso 0.692(5) d P .
C29B C 0.8902(9) 1.0752(16) 0.5792(8) 0.059(2) Uiso 0.308(5) d P .
C30A C 0.9259(4) 1.0694(7) 0.5275(4) 0.063(2) Uiso 0.692(5) d P .
C30B C 0.9374(9) 1.0543(16) 0.5528(9) 0.063(2) Uiso 0.308(5) d P .
C31A C 0.9463(4) 0.9541(7) 0.5393(4) 0.075(2) Uiso 0.692(5) d P .
C31B C 0.9140(9) 1.0008(16) 0.4920(8) 0.075(2) Uiso 0.308(5) d P .
C32A C 0.8961(4) 0.8745(7) 0.5249(3) 0.046(2) Uiso 0.692(5) d P .
C32B C 0.8862(9) 0.8843(15) 0.5064(8) 0.046(2) Uiso 0.308(5) d P .
C33 C 0.8214(2) 0.6862(4) 0.5833(2) 0.0441(12) Uani 1 d . .
H33A H 0.8342(2) 0.6336(4) 0.5607(2) 0.053 Uiso 1 calc R .
C34 C 0.8750(2) 0.7140(4) 0.6279(2) 0.0553(14) Uani 1 d . .
H34A H 0.8644(2) 0.7675(4) 0.6507(2) 0.066 Uiso 1 calc R .
H34B H 0.9049(2) 0.7428(4) 0.6119(2) 0.066 Uiso 1 calc R .
C35 C 0.8997(3) 0.6189(5) 0.6623(2) 0.074(2) Uani 1 d . .
H35A H 0.9164(3) 0.5709(5) 0.6408(2) 0.089 Uiso 1 calc R .
H35B H 0.9310(3) 0.6420(5) 0.6922(2) 0.089 Uiso 1 calc R .
C36 C 0.8549(3) 0.5616(6) 0.6842(2) 0.096(3) Uani 1 d . .
H36A H 0.8719(3) 0.4981(6) 0.7022(2) 0.116 Uiso 1 calc R .
H36B H 0.8425(3) 0.6052(6) 0.7105(2) 0.116 Uiso 1 calc R .
C37 C 0.8033(3) 0.5347(6) 0.6396(3) 0.109(3) Uani 1 d . .
H37A H 0.7740(3) 0.5000(6) 0.6543(3) 0.130 Uiso 1 calc R .
H37B H 0.8153(3) 0.4866(6) 0.6149(3) 0.130 Uiso 1 calc R .
C38 C 0.7774(3) 0.6318(5) 0.6095(2) 0.075(2) Uani 1 d . .
H38A H 0.7656(3) 0.6798(5) 0.6343(2) 0.090 Uiso 1 calc R .
H38B H 0.7429(3) 0.6129(5) 0.5819(2) 0.090 Uiso 1 calc R .
C39 C 0.7356(2) 0.8510(5) 0.5710(2) 0.0597(15) Uani 1 d . .
H39A H 0.7141(2) 0.7936(5) 0.5821(2) 0.072 Uiso 1 calc R .
H39B H 0.7557(2) 0.8881(5) 0.6032(2) 0.072 Uiso 1 calc R .
C40 C 0.6939(2) 0.9226(4) 0.5367(2) 0.0556(14) Uani 1 d . .
H40A H 0.7134(2) 0.9885(4) 0.5336(2) 0.067 Uiso 1 calc R .
H40B H 0.6621(2) 0.9368(4) 0.5537(2) 0.067 Uiso 1 calc R .
C41 C 0.5931(2) 0.8100(4) 0.4742(2) 0.0407(11) Uani 1 d . .
H41A H 0.5793(2) 0.7676(4) 0.4417(2) 0.049 Uiso 1 calc R .
C42 C 0.5436(2) 0.8865(4) 0.4757(2) 0.0512(13) Uani 1 d . .
H42A H 0.5546(2) 0.9294(4) 0.5079(2) 0.061 Uiso 1 calc R .
H42B H 0.5372(2) 0.9324(4) 0.4446(2) 0.061 Uiso 1 calc R .
C43 C 0.4872(2) 0.8277(4) 0.4756(2) 0.0574(15) Uani 1 d . .
H43A H 0.4572(2) 0.8778(4) 0.4786(2) 0.069 Uiso 1 calc R .
H43B H 0.4740(2) 0.7912(4) 0.4416(2) 0.069 Uiso 1 calc R .
C44 C 0.4947(3) 0.7496(4) 0.5211(3) 0.068(2) Uani 1 d . .
H44A H 0.5020(3) 0.7866(4) 0.5552(3) 0.081 Uiso 1 calc R .
H44B H 0.4590(3) 0.7093(4) 0.5173(3) 0.081 Uiso 1 calc R .
C45 C 0.5446(2) 0.6771(4) 0.5210(2) 0.064(2) Uani 1 d . .
H45A H 0.5345(2) 0.6332(4) 0.4892(2) 0.077 Uiso 1 calc R .
H45B H 0.5506(2) 0.6317(4) 0.5523(2) 0.077 Uiso 1 calc R .
C46 C 0.6012(2) 0.7343(4) 0.5217(2) 0.0564(14) Uani 1 d . .
H46A H 0.6314(2) 0.6839(4) 0.5199(2) 0.068 Uiso 1 calc R .
H46B H 0.6136(2) 0.7730(4) 0.5552(2) 0.068 Uiso 1 calc R .
C47 C 0.6509(2) 0.9912(3) 0.4275(2) 0.0466(12) Uani 1 d . .
H47A H 0.6897(2) 1.0090(3) 0.4225(2) 0.056 Uiso 1 calc R .
C48 C 0.6317(3) 1.0895(4) 0.4511(2) 0.068(2) Uani 1 d . .
H48A H 0.6567(3) 1.1016(4) 0.4867(2) 0.082 Uiso 1 calc R .
H48B H 0.5919(3) 1.0809(4) 0.4547(2) 0.082 Uiso 1 calc R .
C49 C 0.6347(3) 1.1831(4) 0.4154(2) 0.071(2) Uani 1 d . .
H49A H 0.6209(3) 1.2450(4) 0.4305(2) 0.086 Uiso 1 calc R .
H49B H 0.6750(3) 1.1951(4) 0.4142(2) 0.086 Uiso 1 calc R .
C50 C 0.5982(3) 1.1655(4) 0.3594(3) 0.086(2) Uani 1 d . .
H50A H 0.5574(3) 1.1617(4) 0.3604(3) 0.103 Uiso 1 calc R .
H50B H 0.6028(3) 1.2248(4) 0.3371(3) 0.103 Uiso 1 calc R .
C51 C 0.6144(3) 1.0675(4) 0.3346(2) 0.070(2) Uani 1 d . .
H51A H 0.6529(3) 1.0759(4) 0.3277(2) 0.085 Uiso 1 calc R .
H51B H 0.5867(3) 1.0553(4) 0.3004(2) 0.085 Uiso 1 calc R .
C52 C 0.6148(2) 0.9733(3) 0.3712(2) 0.0458(12) Uani 1 d . .
H52A H 0.5750(2) 0.9573(3) 0.3726(2) 0.055 Uiso 1 calc R .
H52B H 0.6302(2) 0.9132(3) 0.3560(2) 0.055 Uiso 1 calc R .
B B 0.7264(3) 1.1922(4) 0.7011(2) 0.0462(14) Uani 1 d . .
C53 C 0.7484(2) 1.2660(3) 0.7545(2) 0.0442(12) Uani 1 d . .
C54 C 0.7643(2) 1.3696(4) 0.7537(2) 0.0572(14) Uani 1 d . .
H54A H 0.7618(2) 1.4010(4) 0.7204(2) 0.069 Uiso 1 calc R .
C55 C 0.7839(3) 1.4299(4) 0.7993(3) 0.066(2) Uani 1 d . .
H55A H 0.7942(3) 1.4995(4) 0.7960(3) 0.079 Uiso 1 calc R .
C56 C 0.7882(3) 1.3877(4) 0.8492(2) 0.065(2) Uani 1 d . .
H56A H 0.8006(3) 1.4280(4) 0.8801(2) 0.078 Uiso 1 calc R .
C57 C 0.7739(3) 1.2838(4) 0.8524(2) 0.061(2) Uani 1 d . .
H57A H 0.7770(3) 1.2531(4) 0.8859(2) 0.074 Uiso 1 calc R .
C58 C 0.7548(2) 1.2245(4) 0.8062(2) 0.0546(15) Uani 1 d . .
H58A H 0.7458(2) 1.1543(4) 0.8096(2) 0.065 Uiso 1 calc R .
C59 C 0.6622(2) 1.1418(4) 0.6994(2) 0.0490(13) Uani 1 d . .
C60 C 0.6354(3) 1.0732(4) 0.6575(2) 0.069(2) Uani 1 d . .
H60A H 0.6564(3) 1.0533(4) 0.6327(2) 0.083 Uiso 1 calc R .
C61 C 0.5799(3) 1.0341(5) 0.6512(3) 0.090(3) Uani 1 d . .
H61A H 0.5642(3) 0.9890(5) 0.6229(3) 0.108 Uiso 1 calc R .
C62 C 0.5483(3) 1.0622(6) 0.6868(4) 0.099(3) Uani 1 d . .
H62A H 0.5109(3) 1.0352(6) 0.6831(4) 0.118 Uiso 1 calc R .
C63 C 0.5710(3) 1.1297(5) 0.7279(3) 0.080(2) Uani 1 d . .
H63A H 0.5488(3) 1.1500(5) 0.7517(3) 0.096 Uiso 1 calc R .
C64 C 0.6275(2) 1.1681(4) 0.7341(2) 0.0593(15) Uani 1 d . .
H64A H 0.6425(2) 1.2131(4) 0.7626(2) 0.071 Uiso 1 calc R .
C65 C 0.7786(3) 1.1034(4) 0.7057(2) 0.0536(14) Uani 1 d . .
C66 C 0.7718(3) 0.9955(4) 0.7121(2) 0.063(2) Uani 1 d . .
H66A H 0.7348(3) 0.9696(4) 0.7116(2) 0.075 Uiso 1 calc R .
C67 C 0.8183(4) 0.9258(5) 0.7191(2) 0.085(2) Uani 1 d . .
H67A H 0.8118(4) 0.8547(5) 0.7231(2) 0.102 Uiso 1 calc R .
C68 C 0.8728(4) 0.9600(7) 0.7201(3) 0.095(3) Uani 1 d . .
H68A H 0.9038(4) 0.9133(7) 0.7250(3) 0.114 Uiso 1 calc R .
C69 C 0.8812(3) 1.0635(7) 0.7138(3) 0.102(3) Uani 1 d . .
H69A H 0.9185(3) 1.0880(7) 0.7143(3) 0.123 Uiso 1 calc R .
C70 C 0.8347(3) 1.1342(6) 0.7067(3) 0.084(2) Uani 1 d . .
H70A H 0.8420(3) 1.2049(6) 0.7024(3) 0.101 Uiso 1 calc R .
C71 C 0.7143(3) 1.2597(4) 0.6446(2) 0.060(2) Uani 1 d . .
C72 C 0.6724(3) 1.3391(5) 0.6347(2) 0.072(2) Uani 1 d . .
H72A H 0.6537(3) 1.3568(5) 0.6615(2) 0.087 Uiso 1 calc R .
C73 C 0.6580(4) 1.3921(6) 0.5863(3) 0.101(3) Uani 1 d . .
H73A H 0.6305(4) 1.4457(6) 0.5813(3) 0.122 Uiso 1 calc R .
C74 C 0.6838(5) 1.3663(7) 0.5452(3) 0.119(4) Uani 1 d . .
H74A H 0.6735(5) 1.4013(7) 0.5125(3) 0.143 Uiso 1 calc R .
C75 C 0.7241(5) 1.2899(7) 0.5530(3) 0.113(3) Uani 1 d . .
H75A H 0.7412(5) 1.2712(7) 0.5252(3) 0.136 Uiso 1 calc R .
C76 C 0.7407(3) 1.2381(5) 0.6028(2) 0.079(2) Uani 1 d . .
H76A H 0.7701(3) 1.1879(5) 0.6080(2) 0.095 Uiso 1 calc R .
Cl2 Cl 1.04119(15) 0.7285(4) 0.6225(2) 0.270(3) Uani 1 d . .
Cl3 Cl 1.03569(14) 0.8414(3) 0.71471(13) 0.1793(13) Uani 1 d . .
C77 C 1.0773(4) 0.7775(7) 0.6785(4) 0.129(3) Uani 1 d . .
H77A H 1.1060(4) 0.8262(7) 0.6711(4) 0.155 Uiso 1 calc R .
H77B H 1.0984(4) 0.7215(7) 0.7005(4) 0.155 Uiso 1 calc R .
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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 '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'
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
O1 Os O2 37.92(14) . . ?
O1 Os Cl1 160.15(11) . . ?
O2 Os Cl1 161.65(12) . . ?
O1 Os P4 86.26(10) . . ?
O2 Os P4 84.66(11) . . ?
Cl1 Os P4 97.19(4) . . ?
O1 Os P3 115.14(11) . . ?
O2 Os P3 77.50(12) . . ?
Cl1 Os P3 84.71(4) . . ?
P4 Os P3 81.39(4) . . ?
O1 Os P2 89.72(10) . . ?
O2 Os P2 91.73(11) . . ?
Cl1 Os P2 86.84(4) . . ?
P4 Os P2 175.91(4) . . ?
P3 Os P2 99.73(4) . . ?
O1 Os P1 82.22(11) . . ?
O2 Os P1 120.00(12) . . ?
Cl1 Os P1 77.94(4) . . ?
P4 Os P1 98.11(4) . . ?
P3 Os P1 162.46(4) . . ?
P2 Os P1 82.02(4) . . ?
C13 P1 C1 105.8(2) . . ?
C13 P1 C7 103.8(2) . . ?
C1 P1 C7 104.5(2) . . ?
C13 P1 Os 103.21(15) . . ?
C1 P1 Os 115.05(15) . . ?
C7 P1 Os 122.83(14) . . ?
C14 P2 C15 100.7(2) . . ?
C14 P2 C21 104.7(2) . . ?
C15 P2 C21 105.0(2) . . ?
C14 P2 Os 106.29(15) . . ?
C15 P2 Os 123.0(2) . . ?
C21 P2 Os 114.8(2) . . ?
C39 P3 C27B 106.4(7) . . ?
C39 P3 C33 102.4(2) . . ?
C27B P3 C33 114.0(7) . . ?
C39 P3 C27A 101.6(4) . . ?
C27B P3 C27A 13.3(8) . . ?
C33 P3 C27A 103.7(3) . . ?
C39 P3 Os 106.6(2) . . ?
C27B P3 Os 106.8(7) . . ?
C33 P3 Os 119.7(2) . . ?
C27A P3 Os 120.1(3) . . ?
C40 P4 C41 103.1(2) . . ?
C40 P4 C47 101.2(2) . . ?
C41 P4 C47 110.7(2) . . ?
C40 P4 Os 109.0(2) . . ?
C41 P4 Os 120.17(15) . . ?
C47 P4 Os 110.6(2) . . ?
O2 O1 Os 72.5(2) . . ?
O1 O2 Os 69.6(2) . . ?
C2 C1 C6 110.3(4) . . ?
C2 C1 P1 114.1(3) . . ?
C6 C1 P1 114.6(3) . . ?
C3 C2 C1 111.1(4) . . ?
C4 C3 C2 113.2(4) . . ?
C5 C4 C3 110.4(4) . . ?
C4 C5 C6 111.0(5) . . ?
C5 C6 C1 111.5(4) . . ?
C12 C7 C8 108.6(4) . . ?
C12 C7 P1 118.2(3) . . ?
C8 C7 P1 113.2(3) . . ?
C9 C8 C7 110.9(4) . . ?
C10 C9 C8 111.5(5) . . ?
C9 C10 C11 111.1(5) . . ?
C10 C11 C12 111.5(5) . . ?
C7 C12 C11 110.8(4) . . ?
C14 C13 P1 110.2(3) . . ?
C13 C14 P2 111.8(3) . . ?
C16 C15 C20 107.9(4) . . ?
C16 C15 P2 114.3(3) . . ?
C20 C15 P2 113.7(3) . . ?
C17 C16 C15 112.0(4) . . ?
C16 C17 C18 111.4(5) . . ?
C19 C18 C17 110.7(5) . . ?
C18 C19 C20 111.9(5) . . ?
C19 C20 C15 111.7(5) . . ?
C26 C21 C22 110.3(4) . . ?
C26 C21 P2 114.5(3) . . ?
C22 C21 P2 115.6(3) . . ?
C21 C22 C23 110.7(4) . . ?
C24 C23 C22 111.2(5) . . ?
C23 C24 C25 110.9(5) . . ?
C24 C25 C26 111.5(4) . . ?
C25 C26 C21 111.4(4) . . ?
C28B C27A C32A 114.1(12) . . ?
C28B C27A C28A 58.3(9) . . ?
C32A C27A C28A 113.0(7) . . ?
C28B C27A C32B 121.4(13) . . ?
C32A C27A C32B 16.8(8) . . ?
C28A C27A C32B 102.9(9) . . ?
C28B C27A P3 133.3(11) . . ?
C32A C27A P3 110.3(6) . . ?
C28A C27A P3 115.3(7) . . ?
C32B C27A P3 105.3(8) . . ?
C32A C27B C32B 19.7(9) . . ?
C32A C27B C28A 123.2(17) . . ?
C32B C27B C28A 118.4(18) . . ?
C32A C27B C28B 102.6(15) . . ?
C32B C27B C28B 116.4(18) . . ?
C28A C27B C28B 53.9(10) . . ?
C32A C27B P3 116.7(14) . . ?
C32B C27B P3 117.2(16) . . ?
C28A C27B P3 120.1(15) . . ?
C28B C27B P3 115.0(14) . . ?
C28B C28A C27B 66.5(11) . . ?
C28B C28A C29A 79.2(9) . . ?
C27B C28A C29A 116.9(11) . . ?
C28B C28A C27A 50.8(8) . . ?
C27B C28A C27A 16.3(10) . . ?
C29A C28A C27A 112.4(7) . . ?
C28B C28A C29B 58.9(10) . . ?
C27B C28A C29B 106.6(12) . . ?
C29A C28A C29B 20.4(7) . . ?
C27A C28A C29B 97.7(9) . . ?
C27A C28B C28A 70.9(11) . . ?
C27A C28B C27B 12.3(11) . . ?
C28A C28B C27B 59.6(11) . . ?
C27A C28B C29B 121.6(16) . . ?
C28A C28B C29B 72.1(12) . . ?
C27B C28B C29B 110.9(15) . . ?
C27A C28B C29A 107.7(12) . . ?
C28A C28B C29A 53.5(7) . . ?
C27B C28B C29A 96.0(12) . . ?
C29B C28B C29A 18.8(8) . . ?
C29B C29A C28A 101.4(25) . . ?
C29B C29A C30B 68.8(25) . . ?
C28A C29A C30B 117.5(10) . . ?
C29B C29A C30A 93.3(25) . . ?
C28A C29A C30A 113.6(7) . . ?
C30B C29A C30A 24.5(8) . . ?
C29B C29A C28B 54.5(24) . . ?
C28A C29A C28B 47.3(7) . . ?
C30B C29A C28B 92.1(10) . . ?
C30A C29A C28B 107.0(8) . . ?
C29A C29B C30B 87.8(27) . . ?
C29A C29B C28B 106.8(28) . . ?
C30B C29B C28B 108.8(17) . . ?
C29A C29B C30A 65.7(23) . . ?
C30B C29B C30A 22.1(9) . . ?
C28B C29B C30A 113.3(14) . . ?
C29A C29B C28A 58.1(22) . . ?
C30B C29B C28A 110.0(15) . . ?
C28B C29B C28A 49.0(9) . . ?
C30A C29B C28A 96.2(11) . . ?
C30B C30A C31B 118.2(26) . . ?
C30B C30A C31A 60.3(21) . . ?
C31B C30A C31A 58.6(11) . . ?
C30B C30A C29A 76.2(23) . . ?
C31B C30A C29A 114.6(13) . . ?
C31A C30A C29A 108.1(7) . . ?
C30B C30A C29B 55.2(23) . . ?
C31B C30A C29B 121.4(14) . . ?
C31A C30A C29B 94.4(9) . . ?
C29A C30A C29B 21.0(7) . . ?
C30A C30B C31A 94.3(25) . . ?
C30A C30B C29B 102.7(28) . . ?
C31A C30B C29B 118.2(18) . . ?
C30A C30B C29A 79.3(23) . . ?
C31A C30B C29A 120.8(16) . . ?
C29B C30B C29A 23.4(9) . . ?
C30A C30B C31B 41.1(19) . . ?
C31A C30B C31B 53.9(11) . . ?
C29B C30B C31B 112.9(18) . . ?
C29A C30B C31B 95.1(14) . . ?
C30B C31A C31B 74.5(13) . . ?
C30B C31A C32A 121.9(12) . . ?
C31B C31A C32A 81.3(11) . . ?
C30B C31A C30A 25.4(9) . . ?
C31B C31A C30A 49.4(9) . . ?
C32A C31A C30A 113.3(8) . . ?
C30B C31A C32B 117.2(13) . . ?
C31B C31A C32B 65.4(11) . . ?
C32A C31A C32B 16.2(7) . . ?
C30A C31A C32B 102.5(9) . . ?
C30A C31B C31A 71.9(12) . . ?
C30A C31B C30B 20.7(9) . . ?
C31A C31B C30B 51.6(10) . . ?
C30A C31B C32B 119.3(17) . . ?
C31A C31B C32B 66.2(11) . . ?
C30B C31B C32B 102.4(14) . . ?
C30A C31B C32A 108.0(14) . . ?
C31A C31B C32A 52.5(8) . . ?
C30B C31B C32A 89.7(12) . . ?
C32B C31B C32A 14.1(7) . . ?
C27B C32A C27A 16.5(10) . . ?
C27B C32A C31A 117.1(11) . . ?
C27A C32A C31A 111.5(7) . . ?
C27B C32A C31B 99.7(12) . . ?
C27A C32A C31B 107.4(9) . . ?
C31A C32A C31B 46.2(7) . . ?
C27B C32B C27A 13.6(10) . . ?
C27B C32B C31B 109.0(17) . . ?
C27A C32B C31B 110.7(13) . . ?
C27B C32B C31A 105.6(15) . . ?
C27A C32B C31A 96.4(11) . . ?
C31B C32B C31A 48.3(9) . . ?
C34 C33 C38 107.8(4) . . ?
C34 C33 P3 115.0(3) . . ?
C38 C33 P3 113.8(4) . . ?
C33 C34 C35 112.2(4) . . ?
C36 C35 C34 113.3(5) . . ?
C37 C36 C35 110.1(5) . . ?
C36 C37 C38 110.8(6) . . ?
C37 C38 C33 111.2(6) . . ?
C40 C39 P3 113.5(4) . . ?
C39 C40 P4 112.5(4) . . ?
C42 C41 C46 109.4(4) . . ?
C42 C41 P4 116.5(3) . . ?
C46 C41 P4 111.9(3) . . ?
C43 C42 C41 110.9(4) . . ?
C44 C43 C42 112.5(5) . . ?
C45 C44 C43 110.6(4) . . ?
C44 C45 C46 113.0(5) . . ?
C45 C46 C41 110.8(4) . . ?
C52 C47 C48 110.7(4) . . ?
C52 C47 P4 113.0(3) . . ?
C48 C47 P4 119.6(4) . . ?
C47 C48 C49 110.7(5) . . ?
C50 C49 C48 111.0(5) . . ?
C51 C50 C49 112.6(5) . . ?
C50 C51 C52 111.4(5) . . ?
C47 C52 C51 112.8(4) . . ?
C53 B C59 110.6(4) . . ?
C53 B C71 112.6(4) . . ?
C59 B C71 102.7(4) . . ?
C53 B C65 104.7(4) . . ?
C59 B C65 113.6(4) . . ?
C71 B C65 112.9(5) . . ?
C54 C53 C58 114.2(5) . . ?
C54 C53 B 125.0(5) . . ?
C58 C53 B 120.8(4) . . ?
C53 C54 C55 124.1(5) . . ?
C56 C55 C54 120.2(5) . . ?
C55 C56 C57 118.1(5) . . ?
C56 C57 C58 120.7(6) . . ?
C57 C58 C53 122.7(5) . . ?
C64 C59 C60 114.3(5) . . ?
C64 C59 B 125.1(5) . . ?
C60 C59 B 120.4(5) . . ?
C61 C60 C59 123.6(7) . . ?
C62 C61 C60 119.3(7) . . ?
C61 C62 C63 120.4(7) . . ?
C62 C63 C64 119.8(7) . . ?
C59 C64 C63 122.6(6) . . ?
C70 C65 C66 114.7(6) . . ?
C70 C65 B 120.1(5) . . ?
C66 C65 B 125.1(5) . . ?
C67 C66 C65 122.3(6) . . ?
C68 C67 C66 120.8(7) . . ?
C69 C68 C67 118.7(8) . . ?
C68 C69 C70 120.9(8) . . ?
C65 C70 C69 122.6(7) . . ?
C76 C71 C72 115.8(6) . . ?
C76 C71 B 123.7(6) . . ?
C72 C71 B 120.3(5) . . ?
C73 C72 C71 122.0(7) . . ?
C74 C73 C72 120.6(8) . . ?
C75 C74 C73 119.3(8) . . ?
C74 C75 C76 120.5(9) . . ?
C71 C76 C75 121.8(8) . . ?
Cl2 C77 Cl3 114.8(5) . . ?
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 O1 2.006(3) . ?
Os O2 2.041(4) . ?
Os Cl1 2.3795(11) . ?
Os P4 2.4338(12) . ?
Os P3 2.4802(13) . ?
Os P2 2.4817(12) . ?
Os P1 2.5082(12) . ?
P1 C13 1.839(4) . ?
P1 C1 1.868(5) . ?
P1 C7 1.875(4) . ?
P2 C14 1.831(5) . ?
P2 C15 1.852(5) . ?
P2 C21 1.862(4) . ?
P3 C39 1.830(5) . ?
P3 C27B 1.85(2) . ?
P3 C33 1.869(5) . ?
P3 C27A 1.871(10) . ?
P4 C40 1.846(5) . ?
P4 C41 1.863(5) . ?
P4 C47 1.866(5) . ?
O1 O2 1.315(5) . ?
C1 C2 1.534(6) . ?
C1 C6 1.559(6) . ?
C2 C3 1.533(7) . ?
C3 C4 1.517(7) . ?
C4 C5 1.511(7) . ?
C5 C6 1.524(7) . ?
C7 C12 1.517(7) . ?
C7 C8 1.522(6) . ?
C8 C9 1.515(7) . ?
C9 C10 1.503(8) . ?
C10 C11 1.504(7) . ?
C11 C12 1.543(7) . ?
C13 C14 1.505(6) . ?
C15 C16 1.533(6) . ?
C15 C20 1.545(7) . ?
C16 C17 1.520(7) . ?
C17 C18 1.521(8) . ?
C18 C19 1.517(8) . ?
C19 C20 1.529(7) . ?
C21 C26 1.532(6) . ?
C21 C22 1.537(6) . ?
C22 C23 1.541(6) . ?
C23 C24 1.496(7) . ?
C24 C25 1.510(7) . ?
C25 C26 1.530(6) . ?
C27A C28B 1.26(2) . ?
C27A C32A 1.517(13) . ?
C27A C28A 1.537(12) . ?
C27A C32B 1.67(2) . ?
C27B C32A 1.42(2) . ?
C27B C32B 1.45(3) . ?
C27B C28A 1.48(2) . ?
C27B C28B 1.57(3) . ?
C28A C28B 1.38(2) . ?
C28A C29A 1.512(12) . ?
C28A C29B 1.74(2) . ?
C28B C29B 1.57(3) . ?
C28B C29A 1.85(2) . ?
C29A C29B 0.62(2) . ?
C29A C30B 1.56(2) . ?
C29A C30A 1.581(13) . ?
C29B C30B 1.46(3) . ?
C29B C30A 1.73(2) . ?
C30A C30B 0.67(2) . ?
C30A C31B 1.24(2) . ?
C30A C31A 1.556(13) . ?
C30B C31A 1.36(2) . ?
C30B C31B 1.67(3) . ?
C31A C31B 1.40(2) . ?
C31A C32A 1.536(12) . ?
C31A C32B 1.71(2) . ?
C31B C32B 1.70(3) . ?
C31B C32A 1.91(2) . ?
C33 C34 1.524(6) . ?
C33 C38 1.532(7) . ?
C34 C35 1.531(7) . ?
C35 C36 1.502(9) . ?
C36 C37 1.493(8) . ?
C37 C38 1.508(8) . ?
C39 C40 1.468(7) . ?
C41 C42 1.528(6) . ?
C41 C46 1.529(6) . ?
C42 C43 1.528(7) . ?
C43 C44 1.510(7) . ?
C44 C45 1.498(7) . ?
C45 C46 1.518(7) . ?
C47 C52 1.503(6) . ?
C47 C48 1.508(6) . ?
C48 C49 1.515(7) . ?
C49 C50 1.499(8) . ?
C50 C51 1.493(7) . ?
C51 C52 1.522(6) . ?
B C53 1.637(7) . ?
B C59 1.637(8) . ?
B C71 1.647(8) . ?
B C65 1.656(8) . ?
C53 C54 1.377(6) . ?
C53 C58 1.398(7) . ?
C54 C55 1.380(7) . ?
C55 C56 1.368(8) . ?
C56 C57 1.375(7) . ?
C57 C58 1.384(7) . ?
C59 C64 1.387(7) . ?
C59 C60 1.411(7) . ?
C60 C61 1.372(9) . ?
C61 C62 1.357(11) . ?
C62 C63 1.366(10) . ?
C63 C64 1.391(8) . ?
C65 C70 1.374(8) . ?
C65 C66 1.401(7) . ?
C66 C67 1.390(8) . ?
C67 C68 1.352(10) . ?
C68 C69 1.351(10) . ?
C69 C70 1.398(9) . ?
C71 C76 1.388(8) . ?
C71 C72 1.394(8) . ?
C72 C73 1.381(8) . ?
C73 C74 1.375(11) . ?
C74 C75 1.342(12) . ?
C75 C76 1.406(10) . ?
Cl2 C77 1.606(9) . ?
Cl3 C77 1.710(9) . ?
