# 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_264RKMOs_TW
_database_code_depnum_ccdc_archive 'CCDC 1447861'
_audit_update_record             
;
2016-07-02 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C51 H38 Br N O3 Os P2, I5, 0.5(I2)'
_chemical_formula_sum            'C51 H38 Br I6 N O3 Os P2'
_chemical_formula_weight         1806.27

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   12.0307(4)
_cell_length_b                   15.1139(5)
_cell_length_c                   15.5317(5)
_cell_angle_alpha                73.6450(10)
_cell_angle_beta                 80.7900(10)
_cell_angle_gamma                77.2910(10)
_cell_volume                     2628.91(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    135(2)
_cell_measurement_reflns_used    9873
_cell_measurement_theta_min      2.90
_cell_measurement_theta_max      25.76

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.282
_exptl_crystal_F_000             1668
_exptl_transmission_factor_min   0.208
_exptl_transmission_factor_max   0.512
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    6.811
_shelx_estimated_absorpt_T_min   0.292
_shelx_estimated_absorpt_T_max   0.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      135(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   Mo
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28896
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.858
_diffrn_reflns_theta_max         25.792
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             10031
_reflns_number_gt                9278
_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 (G. M. Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (G. M. Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0379P)²+28.9113P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10031
_refine_ls_number_parameters     596
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1040
_refine_ls_wR_factor_gt          0.1011
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.039
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.51020(2) 0.29510(2) 0.37982(2) 0.01171(7) Uani 1 1 d . . . . .
Br1 Br 0.50158(5) 0.35678(4) 0.51648(4) 0.01801(13) Uani 1 1 d . . . . .
N1 N 0.5244(4) 0.2652(3) 0.2620(3) 0.0152(10) Uani 1 1 d . . . . .
H1 H 0.5068 0.2108 0.2651 0.018 Uiso 1 1 calc R U . . .
C2 C 0.5568(6) 0.3141(5) 0.1767(4) 0.0201(13) Uani 1 1 d . . . . .
C3 C 0.5730(6) 0.2665(5) 0.1079(5) 0.0261(15) Uani 1 1 d . . . . .
H3 H 0.5539 0.2060 0.1214 0.031 Uiso 1 1 calc R U . . .
C4 C 0.6161(7) 0.3071(5) 0.0216(5) 0.0324(17) Uani 1 1 d . . . . .
H4 H 0.6304 0.2733 -0.0234 0.039 Uiso 1 1 calc R U . . .
C5 C 0.6387(7) 0.3977(6) 0.0003(5) 0.0334(17) Uani 1 1 d . . . . .
H5 H 0.6676 0.4256 -0.0595 0.040 Uiso 1 1 calc R U . . .
C6 C 0.6196(6) 0.4475(5) 0.0652(4) 0.0248(14) Uani 1 1 d . . . . .
C7 C 0.6417(7) 0.5451(5) 0.0356(5) 0.0323(17) Uani 1 1 d . . . . .
C8 C 0.6130(7) 0.6015(5) 0.1031(5) 0.0272(15) Uani 1 1 d . . . . .
C9 C 0.6261(8) 0.6945(6) 0.0793(6) 0.042(2) Uani 1 1 d . . . . .
H9 H 0.6547 0.7219 0.0193 0.050 Uiso 1 1 calc R U . . .
C10 C 0.5988(8) 0.7476(6) 0.1407(6) 0.043(2) Uani 1 1 d . . . . .
H10 H 0.6077 0.8114 0.1230 0.051 Uiso 1 1 calc R U . . .
C11 C 0.5578(7) 0.7074(5) 0.2296(6) 0.0349(17) Uani 1 1 d . . . . .
H11 H 0.5386 0.7442 0.2722 0.042 Uiso 1 1 calc R U . . .
C12 C 0.5450(6) 0.6146(5) 0.2556(5) 0.0239(14) Uani 1 1 d . . . . .
H12 H 0.5183 0.5873 0.3162 0.029 Uiso 1 1 calc R U . . .
C13 C 0.5714(5) 0.5612(4) 0.1925(4) 0.0201(13) Uani 1 1 d . . . . .
C14 C 0.5583(5) 0.4626(4) 0.2204(4) 0.0176(12) Uani 1 1 d . . . . .
C15 C 0.5780(5) 0.4074(5) 0.1554(4) 0.0194(13) Uani 1 1 d . . . . .
O17 O 0.6771(6) 0.5788(4) -0.0418(4) 0.0488(16) Uani 1 1 d . . . . .
O16 O 0.5283(3) 0.4305(3) 0.3032(3) 0.0138(8) Uani 1 1 d . . . . .
C18 C 0.4905(5) 0.1697(5) 0.4416(4) 0.0171(12) Uani 1 1 d . U . . .
O19 O 0.4736(4) 0.1005(3) 0.4779(3) 0.0284(11) Uani 1 1 d . . . . .
P20 P 0.30342(12) 0.34132(10) 0.38484(10) 0.0122(3) Uani 1 1 d . . . . .
C21 C 0.2209(5) 0.3242(4) 0.4954(4) 0.0159(12) Uani 1 1 d . . . . .
C22 C 0.1081(5) 0.3726(5) 0.5018(5) 0.0219(13) Uani 1 1 d . . . . .
H22 H 0.0785 0.4165 0.4500 0.026 Uiso 1 1 calc R U . . .
C23 C 0.0388(6) 0.3574(5) 0.5827(5) 0.0284(16) Uani 1 1 d . . . . .
H23 H -0.0377 0.3911 0.5866 0.034 Uiso 1 1 calc R U . . .
C24 C 0.0825(6) 0.2917(5) 0.6595(5) 0.0275(15) Uani 1 1 d . . . . .
H24 H 0.0352 0.2803 0.7151 0.033 Uiso 1 1 calc R U . . .
C25 C 0.1938(6) 0.2441(5) 0.6535(5) 0.0230(14) Uani 1 1 d . . . . .
H25 H 0.2233 0.2006 0.7057 0.028 Uiso 1 1 calc R U . . .
C26 C 0.2639(5) 0.2587(4) 0.5720(4) 0.0186(13) Uani 1 1 d . . . . .
H26 H 0.3402 0.2246 0.5683 0.022 Uiso 1 1 calc R U . . .
C31 C 0.2428(5) 0.2747(4) 0.3286(4) 0.0154(12) Uani 1 1 d . . . . .
C32 C 0.1812(6) 0.2059(5) 0.3792(5) 0.0233(14) Uani 1 1 d . . . . .
H32 H 0.1663 0.1968 0.4428 0.028 Uiso 1 1 calc R U . . .
C33 C 0.1413(6) 0.1504(5) 0.3373(5) 0.0310(16) Uani 1 1 d . . . . .
H33 H 0.1004 0.1030 0.3724 0.037 Uiso 1 1 calc R U . . .
C34 C 0.1611(7) 0.1644(5) 0.2451(6) 0.0334(17) Uani 1 1 d . . . . .
H34 H 0.1328 0.1271 0.2165 0.040 Uiso 1 1 calc R U . . .
C35 C 0.2216(6) 0.2323(5) 0.1940(5) 0.0258(14) Uani 1 1 d . . . . .
H35 H 0.2348 0.2418 0.1304 0.031 Uiso 1 1 calc R U . . .
C36 C 0.2635(6) 0.2870(5) 0.2352(4) 0.0215(13) Uani 1 1 d . . . . .
H36 H 0.3064 0.3329 0.1998 0.026 Uiso 1 1 calc R U . . .
C41 C 0.2632(5) 0.4669(4) 0.3345(4) 0.0149(12) Uani 1 1 d . . . . .
C42 C 0.2149(5) 0.5062(4) 0.2533(4) 0.0198(13) Uani 1 1 d . . . . .
H42 H 0.1963 0.4669 0.2217 0.024 Uiso 1 1 calc R U . . .
C43 C 0.1939(6) 0.6041(5) 0.2182(5) 0.0230(14) Uani 1 1 d . . . . .
H43 H 0.1614 0.6313 0.1627 0.028 Uiso 1 1 calc R U . . .
C44 C 0.2206(5) 0.6604(5) 0.2647(5) 0.0230(14) Uani 1 1 d . . . . .
H44 H 0.2067 0.7265 0.2407 0.028 Uiso 1 1 calc R U . . .
C45 C 0.2673(6) 0.6224(5) 0.3456(5) 0.0232(14) Uani 1 1 d . . . . .
H45 H 0.2848 0.6622 0.3773 0.028 Uiso 1 1 calc R U . . .
C46 C 0.2886(5) 0.5259(4) 0.3806(5) 0.0206(13) Uani 1 1 d . . . . .
H46 H 0.3208 0.4997 0.4364 0.025 Uiso 1 1 calc R U . . .
P50 P 0.71736(13) 0.25377(11) 0.38413(10) 0.0146(3) Uani 1 1 d . . . . .
C51 C 0.7927(5) 0.3514(4) 0.3381(4) 0.0186(13) Uani 1 1 d . . . . .
C52 C 0.7496(6) 0.4337(5) 0.3669(5) 0.0235(14) Uani 1 1 d . . . . .
H52 H 0.6813 0.4376 0.4070 0.028 Uiso 1 1 calc R U . . .
C53 C 0.8062(7) 0.5093(5) 0.3370(5) 0.0319(16) Uani 1 1 d . . . . .
H53 H 0.7771 0.5646 0.3572 0.038 Uiso 1 1 calc R U . . .
C54 C 0.9054(7) 0.5041(6) 0.2778(5) 0.0340(17) Uani 1 1 d . . . . .
H54 H 0.9434 0.5562 0.2564 0.041 Uiso 1 1 calc R U . . .
C55 C 0.9490(6) 0.4227(6) 0.2501(5) 0.0335(17) Uani 1 1 d . . . . .
H55 H 1.0171 0.4193 0.2098 0.040 Uiso 1 1 calc R U . . .
C56 C 0.8945(5) 0.3465(5) 0.2804(5) 0.0229(14) Uani 1 1 d . . . . .
H56 H 0.9263 0.2905 0.2619 0.028 Uiso 1 1 calc R U . . .
C61 C 0.7786(5) 0.1655(5) 0.3216(5) 0.0225(14) Uani 1 1 d . . . . .
C62 C 0.8022(6) 0.1897(7) 0.2284(6) 0.0382(19) Uani 1 1 d . . . . .
H62 H 0.7915 0.2539 0.1959 0.046 Uiso 1 1 calc R U . . .
C63 C 0.8418(7) 0.1197(10) 0.1825(8) 0.066(4) Uani 1 1 d . . . . .
H63 H 0.8599 0.1360 0.1189 0.079 Uiso 1 1 calc R U . . .
C64 C 0.8544(8) 0.0260(9) 0.2304(10) 0.067(4) Uani 1 1 d . . . . .
H64 H 0.8814 -0.0218 0.1994 0.080 Uiso 1 1 calc R U . . .
C65 C 0.8288(9) 0.0030(7) 0.3202(9) 0.063(3) Uani 1 1 d . . . . .
H65 H 0.8355 -0.0614 0.3518 0.076 Uiso 1 1 calc R U . . .
C66 C 0.7922(7) 0.0717(6) 0.3682(7) 0.040(2) Uani 1 1 d . . . . .
H66 H 0.7770 0.0543 0.4321 0.048 Uiso 1 1 calc R U . . .
C71 C 0.7699(5) 0.2004(4) 0.4941(4) 0.0173(12) Uani 1 1 d . . . . .
C72 C 0.7047(6) 0.1508(5) 0.5671(5) 0.0272(15) Uani 1 1 d . . . . .
H72 H 0.6276 0.1490 0.5623 0.033 Uiso 1 1 calc R U . . .
C73 C 0.7535(7) 0.1040(6) 0.6470(5) 0.0342(17) Uani 1 1 d . . . . .
H73 H 0.7101 0.0689 0.6960 0.041 Uiso 1 1 calc R U . . .
C74 C 0.8641(7) 0.1083(5) 0.6553(5) 0.0330(17) Uani 1 1 d . . . . .
H74 H 0.8969 0.0763 0.7100 0.040 Uiso 1 1 calc R U . . .
C75 C 0.9270(7) 0.1587(6) 0.5849(5) 0.0328(17) Uani 1 1 d . . . . .
H75 H 1.0029 0.1624 0.5915 0.039 Uiso 1 1 calc R U . . .
C76 C 0.8813(6) 0.2045(5) 0.5040(5) 0.0276(15) Uani 1 1 d . . . . .
H76 H 0.9262 0.2387 0.4554 0.033 Uiso 1 1 calc R U . . .
I1 I 0.52459(5) 0.00486(4) 1.27904(4) 0.04167(14) Uani 1 1 d . . . . .
I2 I 0.60884(5) 0.01713(3) 1.09713(4) 0.03655(13) Uani 1 1 d . . . . .
I3 I 0.70034(8) 0.04233(11) 0.89973(6) 0.0526(3) Uani 0.914(4) 1 d D . P A 1
I4 I 0.89922(10) 0.11906(7) 0.92055(5) 0.0371(2) Uani 0.914(4) 1 d D . P A 1
I5 I 1.08665(12) 0.19684(6) 0.93904(6) 0.0516(2) Uani 0.914(4) 1 d D . P A 1
I3' I 0.6832(8) -0.0003(11) 0.9198(7) 0.0526(3) Uani 0.086(4) 1 d D . P A 2
I4' I 0.8703(9) 0.0967(8) 0.9314(7) 0.0371(2) Uani 0.086(4) 1 d D . P A 2
I5' I 1.0468(11) 0.1949(8) 0.9295(8) 0.0516(2) Uani 0.086(4) 1 d D . P A 2
I6 I 1.01297(6) 0.41161(5) 0.98749(5) 0.05716(18) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C18 1.915(6) . ?
Os1 N1 1.978(5) . ?
Os1 O16 2.096(4) . ?
Os1 P20 2.4262(15) . ?
Os1 P50 2.4394(15) . ?
Os1 Br1 2.5272(6) . ?
N1 C2 1.365(8) . ?
N1 H1 0.8800 . ?
C2 C3 1.416(9) . ?
C2 C15 1.425(9) . ?
C3 C4 1.377(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.383(10) . ?
C5 H5 0.9500 . ?
C6 C15 1.419(9) . ?
C6 C7 1.487(10) . ?
C7 O17 1.213(9) . ?
C7 C8 1.484(11) . ?
C8 C9 1.387(11) . ?
C8 C13 1.409(9) . ?
C9 C10 1.369(12) . ?
C9 H9 0.9500 . ?
C10 C11 1.400(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.394(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.467(9) . ?
C14 O16 1.263(7) . ?
C14 C15 1.442(9) . ?
C18 O19 1.085(8) . ?
P20 C21 1.821(6) . ?
P20 C41 1.825(6) . ?
P20 C31 1.825(6) . ?
C21 C22 1.396(9) . ?
C21 C26 1.404(9) . ?
C22 C23 1.383(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.410(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(10) . ?
C24 H24 0.9500 . ?
C25 C26 1.395(9) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.392(9) . ?
C31 C36 1.398(9) . ?
C32 C33 1.394(10) . ?
C32 H32 0.9500 . ?
C33 C34 1.377(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.378(11) . ?
C34 H34 0.9500 . ?
C35 C36 1.390(10) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.394(9) . ?
C41 C46 1.397(9) . ?
C42 C43 1.406(9) . ?
C42 H42 0.9500 . ?
C43 C44 1.374(10) . ?
C43 H43 0.9500 . ?
C44 C45 1.380(10) . ?
C44 H44 0.9500 . ?
C45 C46 1.386(9) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
P50 C51 1.816(6) . ?
P50 C71 1.820(6) . ?
P50 C61 1.826(7) . ?
C51 C56 1.399(9) . ?
C51 C52 1.403(9) . ?
C52 C53 1.389(10) . ?
C52 H52 0.9500 . ?
C53 C54 1.387(11) . ?
C53 H53 0.9500 . ?
C54 C55 1.384(12) . ?
C54 H54 0.9500 . ?
C55 C56 1.381(10) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C66 1.386(11) . ?
C61 C62 1.387(11) . ?
C62 C63 1.396(13) . ?
C62 H62 0.9500 . ?
C63 C64 1.389(18) . ?
C63 H63 0.9500 . ?
C64 C65 1.340(18) . ?
C64 H64 0.9500 . ?
C65 C66 1.401(12) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 C76 1.390(9) . ?
C71 C72 1.399(9) . ?
C72 C73 1.393(10) . ?
C72 H72 0.9500 . ?
C73 C74 1.374(11) . ?
C73 H73 0.9500 . ?
C74 C75 1.367(11) . ?
C74 H74 0.9500 . ?
C75 C76 1.387(10) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
I1 I2 2.8134(8) . ?
I2 I3' 2.824(9) . ?
I2 I3 3.0338(11) . ?
I3 I4 2.9756(11) . ?
I4 I5 2.8483(11) . ?
I3' I4' 2.996(8) . ?
I4' I5' 2.838(8) . ?
I6 I6 2.7508(15) 2_767 ?

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
C18 Os1 N1 90.6(2) . . ?
C18 Os1 O16 175.5(2) . . ?
N1 Os1 O16 85.18(18) . . ?
C18 Os1 P20 88.72(17) . . ?
N1 Os1 P20 92.98(15) . . ?
O16 Os1 P20 90.04(11) . . ?
C18 Os1 P50 92.13(17) . . ?
N1 Os1 P50 91.18(15) . . ?
O16 Os1 P50 89.42(12) . . ?
P20 Os1 P50 175.74(5) . . ?
C18 Os1 Br1 98.16(19) . . ?
N1 Os1 Br1 171.13(15) . . ?
O16 Os1 Br1 86.11(11) . . ?
P20 Os1 Br1 88.69(4) . . ?
P50 Os1 Br1 87.06(4) . . ?
C2 N1 Os1 131.3(4) . . ?
C2 N1 H1 114.3 . . ?
Os1 N1 H1 114.3 . . ?
N1 C2 C3 116.7(6) . . ?
N1 C2 C15 123.5(6) . . ?
C3 C2 C15 119.8(6) . . ?
C4 C3 C2 120.6(7) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 120.0(7) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.8(7) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C15 121.0(7) . . ?
C5 C6 C7 117.1(6) . . ?
C15 C6 C7 121.8(6) . . ?
O17 C7 C8 121.3(7) . . ?
O17 C7 C6 121.3(7) . . ?
C8 C7 C6 117.4(6) . . ?
C9 C8 C13 118.9(7) . . ?
C9 C8 C7 120.7(7) . . ?
C13 C8 C7 120.3(6) . . ?
C10 C9 C8 121.4(7) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C9 C10 C11 119.6(7) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C12 C11 C10 120.3(7) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 119.7(7) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C8 120.0(6) . . ?
C12 C13 C14 119.6(6) . . ?
C8 C13 C14 120.4(6) . . ?
O16 C14 C15 123.1(6) . . ?
O16 C14 C13 116.1(6) . . ?
C15 C14 C13 120.8(6) . . ?
C6 C15 C2 117.6(6) . . ?
C6 C15 C14 119.0(6) . . ?
C2 C15 C14 123.4(6) . . ?
C14 O16 Os1 132.0(4) . . ?
O19 C18 Os1 176.3(6) . . ?
C21 P20 C41 103.5(3) . . ?
C21 P20 C31 102.8(3) . . ?
C41 P20 C31 110.4(3) . . ?
C21 P20 Os1 117.6(2) . . ?
C41 P20 Os1 110.47(19) . . ?
C31 P20 Os1 111.54(19) . . ?
C22 C21 C26 119.3(6) . . ?
C22 C21 P20 118.3(5) . . ?
C26 C21 P20 122.1(5) . . ?
C23 C22 C21 120.8(6) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 119.6(6) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
C25 C24 C23 119.8(6) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 120.8(6) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C21 119.6(6) . . ?
C25 C26 H26 120.2 . . ?
C21 C26 H26 120.2 . . ?
C32 C31 C36 118.8(6) . . ?
C32 C31 P20 120.2(5) . . ?
C36 C31 P20 120.9(5) . . ?
C31 C32 C33 120.5(6) . . ?
C31 C32 H32 119.8 . . ?
C33 C32 H32 119.8 . . ?
C34 C33 C32 120.0(7) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C35 120.2(7) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 C36 120.3(7) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C31 120.2(6) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C42 C41 C46 119.2(6) . . ?
C42 C41 P20 124.9(5) . . ?
C46 C41 P20 115.8(5) . . ?
C41 C42 C43 119.9(6) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 H42 120.1 . . ?
C44 C43 C42 119.6(6) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C45 121.1(6) . . ?
C43 C44 H44 119.5 . . ?
C45 C44 H44 119.5 . . ?
C44 C45 C46 119.7(6) . . ?
C44 C45 H45 120.1 . . ?
C46 C45 H45 120.1 . . ?
C45 C46 C41 120.5(6) . . ?
C45 C46 H46 119.8 . . ?
C41 C46 H46 119.8 . . ?
C51 P50 C71 103.0(3) . . ?
C51 P50 C61 107.4(3) . . ?
C71 P50 C61 103.1(3) . . ?
C51 P50 Os1 114.7(2) . . ?
C71 P50 Os1 117.3(2) . . ?
C61 P50 Os1 110.2(2) . . ?
C56 C51 C52 118.8(6) . . ?
C56 C51 P50 123.3(5) . . ?
C52 C51 P50 117.7(5) . . ?
C53 C52 C51 120.4(6) . . ?
C53 C52 H52 119.8 . . ?
C51 C52 H52 119.8 . . ?
C54 C53 C52 119.9(7) . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C55 C54 C53 119.9(7) . . ?
C55 C54 H54 120.1 . . ?
C53 C54 H54 120.1 . . ?
C56 C55 C54 120.8(7) . . ?
C56 C55 H55 119.6 . . ?
C54 C55 H55 119.6 . . ?
C55 C56 C51 120.2(7) . . ?
C55 C56 H56 119.9 . . ?
C51 C56 H56 119.9 . . ?
C66 C61 C62 119.6(7) . . ?
C66 C61 P50 118.4(6) . . ?
C62 C61 P50 121.7(6) . . ?
C61 C62 C63 119.9(10) . . ?
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C64 C63 C62 119.6(10) . . ?
C64 C63 H63 120.2 . . ?
C62 C63 H63 120.2 . . ?
C65 C64 C63 120.2(9) . . ?
C65 C64 H64 119.9 . . ?
C63 C64 H64 119.9 . . ?
C64 C65 C66 121.4(11) . . ?
C64 C65 H65 119.3 . . ?
C66 C65 H65 119.3 . . ?
C61 C66 C65 119.2(10) . . ?
C61 C66 H66 120.4 . . ?
C65 C66 H66 120.4 . . ?
C76 C71 C72 119.0(6) . . ?
C76 C71 P50 118.5(5) . . ?
C72 C71 P50 122.4(5) . . ?
C73 C72 C71 119.7(7) . . ?
C73 C72 H72 120.2 . . ?
C71 C72 H72 120.2 . . ?
C74 C73 C72 120.4(7) . . ?
C74 C73 H73 119.8 . . ?
C72 C73 H73 119.8 . . ?
C75 C74 C73 120.0(7) . . ?
C75 C74 H74 120.0 . . ?
C73 C74 H74 120.0 . . ?
C74 C75 C76 120.7(7) . . ?
C74 C75 H75 119.6 . . ?
C76 C75 H75 119.6 . . ?
C75 C76 C71 120.1(7) . . ?
C75 C76 H76 120.0 . . ?
C71 C76 H76 120.0 . . ?
I1 I2 I3' 170.4(3) . . ?
I1 I2 I3 176.64(4) . . ?
I4 I3 I2 93.06(3) . . ?
I5 I4 I3 178.66(4) . . ?
I2 I3' I4' 84.4(3) . . ?
I5' I4' I3' 176.0(5) . . ?

_refine_diff_density_max         2.556
_refine_diff_density_min         -2.346
_refine_diff_density_rms         0.196

_shelxl_version_number           2013-2


# start Validation Reply Form
_vrf_PLAT973_264RKMOs_TW         
;
PROBLEM: Check Calcd Positive Residual Density on     Os1       2.19 eA-3  
RESPONSE: The structure suffers from slight disorder of
the complex cation and the I5- anionic unit. Five relatively
small residual density peaks (2.56-2.02 eA^-3) are located
in close vicinity (0.42-0.96 A) to the Osmium and Iodine atoms
;
_vrf_PLAT910_264RKMOs_TW         
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          15 Note  
RESPONSE: 15 reflections at low angles were shaded by 
the beam stopper and were excluded from the refinement
 since they had zero intensity or very low intensity
;
_vrf_PLAT971_264RKMOs_TW         
;
PROBLEM: Check Calcd Residual Density  0.92A From      I3       2.60 eA-3  
RESPONSE: The structure suffers from slight disorder of
the complex cation and the I5- anionic unit. Five relatively
small residual density peaks (2.56-2.02 eA^-3) are located
in close vicinity (0.42-0.96 A) to the Osmium and Iodine atoms
;
####################################################################### 
# 
# 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_8394
_database_code_depnum_ccdc_archive 'CCDC 1447862'
_audit_update_record             
;
2016-07-02 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_audit_creation_date             2013-08-19
_audit_block_code                FNG-PG-510-09
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_compound_source        toluene
_chemical_formula_moiety         'C51 H38.5 Br N O3 Os P2, 1.25(C7 H8)'
_chemical_formula_sum            'C59.75 H48.5 Br N O3 Os P2'
_chemical_formula_weight         1160.54

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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/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                   15.239(3)
_cell_length_b                   24.074(5)
_cell_length_c                   26.860(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.596(4)
_cell_angle_gamma                90
_cell_volume                     9853(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9330
_cell_measurement_theta_min      2.4271
_cell_measurement_theta_max      30.3850

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_F_000             4632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    3.512
_shelx_estimated_absorpt_T_min   0.368
_shelx_estimated_absorpt_T_max   0.872
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_absorpt_correction_T_min  0.55733
_exptl_absorpt_correction_T_max  0.88415

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_detector_area_resol_mean 66.67
_diffrn_reflns_number            287604
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_av_R_equivalents  0.0966
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.136
_diffrn_reflns_theta_max         31.131
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             31509
_reflns_number_gt                23776
_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       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.

 The minimum and maximum estimated transmissions from the multi-scan
 scaling are 0.5764 and 0.9008 (SADABS).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0178P)²+13.3789P]
 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         31509
_refine_ls_number_parameters     1257
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0673
_refine_ls_wR_factor_gt          0.0599
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.003
_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
Os1 Os -0.66524(2) 0.18280(2) 0.69039(2) 0.01083(2) Uani 1 1 d . . . . .
Br1 Br -0.65838(2) 0.18662(2) 0.78646(2) 0.01455(5) Uani 1 1 d . . . . .
N1 N -0.65095(14) 0.18703(10) 0.61518(8) 0.0131(4) Uani 1 1 d . . . . .
H1 H -0.6919 0.1700 0.5977 0.016 Uiso 1 1 calc R U . . .
C2 C -0.58911(17) 0.21165(11) 0.58861(10) 0.0133(5) Uani 1 1 d . . . . .
C3 C -0.60279(18) 0.21528(12) 0.53533(10) 0.0153(5) Uani 1 1 d . . . . .
H3 H -0.6522 0.1971 0.5209 0.018 Uiso 1 1 calc R U . . .
C4 C -0.54759(19) 0.24365(12) 0.50536(10) 0.0176(6) Uani 1 1 d . . . . .
H4 H -0.5612 0.2477 0.4709 0.021 Uiso 1 1 calc R U . . .
C5 C -0.46953(18) 0.26739(12) 0.52522(10) 0.0170(6) Uani 1 1 d . . . . .
H5 H -0.4306 0.2866 0.5038 0.020 Uiso 1 1 calc R U . . .
C6 C -0.44964(17) 0.26292(12) 0.57501(10) 0.0144(5) Uani 1 1 d . . . . .
C7 C -0.36326(18) 0.28460(12) 0.59229(10) 0.0154(5) Uani 1 1 d . . . . .
C8 C -0.34661(17) 0.28620(12) 0.64652(10) 0.0145(5) Uani 1 1 d . . . . .
C9 C -0.26888(18) 0.31026(12) 0.66515(11) 0.0195(6) Uani 1 1 d . . . . .
H9 H -0.2268 0.3247 0.6427 0.023 Uiso 1 1 calc R U . . .
C10 C -0.25327(19) 0.31308(13) 0.71594(11) 0.0208(6) Uani 1 1 d . . . . .
H10 H -0.2016 0.3305 0.7284 0.025 Uiso 1 1 calc R U . . .
C11 C -0.31341(19) 0.29034(13) 0.74875(11) 0.0209(6) Uani 1 1 d . . . . .
H11 H -0.3021 0.2916 0.7836 0.025 Uiso 1 1 calc R U . . .
C12 C -0.38998(18) 0.26582(13) 0.73083(11) 0.0187(6) Uani 1 1 d . . . . .
H12 H -0.4304 0.2502 0.7536 0.022 Uiso 1 1 calc R U . . .
C13 C -0.40829(17) 0.26390(12) 0.67960(10) 0.0141(5) Uani 1 1 d . . . . .
C14 C -0.49118(17) 0.23842(11) 0.66122(10) 0.0123(5) Uani 1 1 d . . . . .
C15 C -0.50993(17) 0.23669(11) 0.60942(10) 0.0126(5) Uani 1 1 d . . . . .
O16 O -0.54104(12) 0.21967(8) 0.69568(7) 0.0148(4) Uani 1 1 d . . . . .
O17 O -0.30711(13) 0.30033(9) 0.56263(8) 0.0212(5) Uani 1 1 d . . . . .
C21 C -0.77367(18) 0.14904(12) 0.68622(10) 0.0145(5) Uani 1 1 d . . . . .
O22 O -0.84157(13) 0.12703(9) 0.68228(8) 0.0208(4) Uani 1 1 d . . . . .
P30 P -0.73217(5) 0.27339(3) 0.68761(3) 0.01317(14) Uani 1 1 d . . . . .
C31 C -0.84806(18) 0.27315(12) 0.70599(10) 0.0156(6) Uani 1 1 d . . . . .
C32 C -0.9119(2) 0.30649(13) 0.68358(11) 0.0217(6) Uani 1 1 d . . . . .
H32 H -0.8961 0.3306 0.6572 0.026 Uiso 1 1 calc R U . . .
C33 C -0.9985(2) 0.30480(14) 0.69945(12) 0.0251(7) Uani 1 1 d . . . . .
H33 H -1.0417 0.3273 0.6836 0.030 Uiso 1 1 calc R U . . .
C34 C -1.02185(19) 0.27012(14) 0.73858(11) 0.0230(7) Uani 1 1 d . . . . .
H34 H -1.0809 0.2688 0.7495 0.028 Uiso 1 1 calc R U . . .
C35 C -0.95839(18) 0.23748(13) 0.76154(11) 0.0188(6) Uani 1 1 d . . . . .
H35 H -0.9743 0.2139 0.7883 0.023 Uiso 1 1 calc R U . . .
C36 C -0.87167(18) 0.23892(12) 0.74584(10) 0.0173(6) Uani 1 1 d . . . . .
H36 H -0.8286 0.2167 0.7621 0.021 Uiso 1 1 calc R U . . .
C41 C -0.73179(18) 0.30263(11) 0.62466(10) 0.0150(5) Uani 1 1 d . . . . .
C42 C -0.66300(19) 0.33745(12) 0.61044(11) 0.0181(6) Uani 1 1 d . . . . .
H42 H -0.6205 0.3490 0.6344 0.022 Uiso 1 1 calc R U . . .
C43 C -0.6564(2) 0.35544(13) 0.56103(11) 0.0218(6) Uani 1 1 d . . . . .
H43 H -0.6092 0.3788 0.5516 0.026 Uiso 1 1 calc R U . . .
C44 C -0.7186(2) 0.33924(13) 0.52584(11) 0.0228(7) Uani 1 1 d . . . . .
H44 H -0.7149 0.3522 0.4925 0.027 Uiso 1 1 calc R U . . .
C45 C -0.7865(2) 0.30377(13) 0.53974(11) 0.0217(6) Uani 1 1 d . . . . .
H45 H -0.8289 0.2922 0.5157 0.026 Uiso 1 1 calc R U . . .
C46 C -0.79242(19) 0.28531(13) 0.58848(11) 0.0189(6) Uani 1 1 d . . . . .
H46 H -0.8382 0.2606 0.5974 0.023 Uiso 1 1 calc R U . . .
C51 C -0.68674(18) 0.33119(12) 0.72446(10) 0.0162(6) Uani 1 1 d . . . . .
C52 C -0.7320(2) 0.38180(14) 0.72519(12) 0.0263(7) Uani 1 1 d . . . . .
H52 H -0.7861 0.3853 0.7075 0.032 Uiso 1 1 calc R U . . .
C53 C -0.6987(2) 0.42708(14) 0.75150(13) 0.0305(8) Uani 1 1 d . . . . .
H53 H -0.7302 0.4611 0.7521 0.037 Uiso 1 1 calc R U . . .
C54 C -0.6197(2) 0.42238(14) 0.77678(12) 0.0291(8) Uani 1 1 d . . . . .
H54 H -0.5967 0.4533 0.7946 0.035 Uiso 1 1 calc R U . . .
C55 C -0.5737(2) 0.37258(14) 0.77615(12) 0.0266(7) Uani 1 1 d . . . . .
H55 H -0.5190 0.3696 0.7932 0.032 Uiso 1 1 calc R U . . .
C56 C -0.6078(2) 0.32709(13) 0.75043(11) 0.0200(6) Uani 1 1 d . . . . .
H56 H -0.5767 0.2929 0.7507 0.024 Uiso 1 1 calc R U . . .
P60 P -0.59600(4) 0.09408(3) 0.69313(3) 0.01319(14) Uani 1 1 d . . . . .
C61 C -0.59512(19) 0.05530(12) 0.63428(10) 0.0163(6) Uani 1 1 d . . . . .
C62 C -0.6713(2) 0.05566(13) 0.60461(11) 0.0199(6) Uani 1 1 d . . . . .
H62 H -0.7199 0.0777 0.6144 0.024 Uiso 1 1 calc R U . . .
C63 C -0.6769(2) 0.02441(13) 0.56114(12) 0.0248(7) Uani 1 1 d . . . . .
H63 H -0.7294 0.0249 0.5418 0.030 Uiso 1 1 calc R U . . .
C64 C -0.6065(2) -0.00747(14) 0.54598(12) 0.0280(7) Uani 1 1 d . . . . .
H64 H -0.6102 -0.0285 0.5161 0.034 Uiso 1 1 calc R U . . .
C65 C -0.5302(2) -0.00835(14) 0.57499(12) 0.0267(7) Uani 1 1 d . . . . .
H65 H -0.4816 -0.0302 0.5649 0.032 Uiso 1 1 calc R U . . .
C66 C -0.5245(2) 0.02248(13) 0.61859(11) 0.0224(6) Uani 1 1 d . . . . .
H66 H -0.4721 0.0213 0.6381 0.027 Uiso 1 1 calc R U . . .
C71 C -0.48164(18) 0.10052(12) 0.71308(10) 0.0162(6) Uani 1 1 d . . . . .
C72 C -0.41559(19) 0.11510(13) 0.67991(11) 0.0204(6) Uani 1 1 d . . . . .
H72 H -0.4285 0.1176 0.6453 0.024 Uiso 1 1 calc R U . . .
C73 C -0.3307(2) 0.12605(14) 0.69722(12) 0.0261(7) Uani 1 1 d . . . . .
H73 H -0.2858 0.1352 0.6743 0.031 Uiso 1 1 calc R U . . .
C74 C -0.3117(2) 0.12362(15) 0.74783(13) 0.0305(8) Uani 1 1 d . . . . .
H74 H -0.2537 0.1305 0.7595 0.037 Uiso 1 1 calc R U . . .
C75 C -0.3768(2) 0.11125(16) 0.78100(12) 0.0309(8) Uani 1 1 d . . . . .
H75 H -0.3640 0.1109 0.8157 0.037 Uiso 1 1 calc R U . . .
C76 C -0.4620(2) 0.09921(14) 0.76421(11) 0.0249(7) Uani 1 1 d . . . . .
H76 H -0.5064 0.0902 0.7874 0.030 Uiso 1 1 calc R U . . .
C81 C -0.64050(19) 0.04151(12) 0.73556(10) 0.0176(6) Uani 1 1 d . . . . .
C82 C -0.5972(2) -0.00959(14) 0.73949(12) 0.0285(8) Uani 1 1 d . . . . .
H82 H -0.5455 -0.0159 0.7209 0.034 Uiso 1 1 calc R U . . .
C83 C -0.6289(2) -0.05124(15) 0.77024(13) 0.0337(8) Uani 1 1 d . . . . .
H83 H -0.5987 -0.0856 0.7730 0.040 Uiso 1 1 calc R U . . .
C84 C -0.7053(2) -0.04208(14) 0.79695(12) 0.0291(8) Uani 1 1 d . . . . .
H84 H -0.7280 -0.0706 0.8176 0.035 Uiso 1 1 calc R U . . .
C85 C -0.7480(2) 0.00808(13) 0.79354(11) 0.0243(7) Uani 1 1 d . . . . .
H85 H -0.7997 0.0142 0.8122 0.029 Uiso 1 1 calc R U . . .
C86 C -0.71622(19) 0.05005(12) 0.76305(10) 0.0182(6) Uani 1 1 d . . . . .
H86 H -0.7462 0.0846 0.7610 0.022 Uiso 1 1 calc R U . . .
Os2 Os -0.16114(2) 0.28423(2) 0.42835(2) 0.01080(2) Uani 1 1 d . . . . .
Br2 Br -0.15525(2) 0.29622(2) 0.33316(2) 0.01471(5) Uani 1 1 d . . . . .
N101 N -0.14943(14) 0.26639(10) 0.50212(8) 0.0149(5) Uani 1 1 d . . . . .
H101 H -0.1924 0.2790 0.5206 0.018 Uiso 1 1 calc R U . . .
C102 C -0.08790(18) 0.23904(12) 0.52680(10) 0.0158(6) Uani 1 1 d . . . . .
C103 C -0.1006(2) 0.23053(14) 0.57979(11) 0.0225(7) Uani 1 1 d . . . . .
H103 H -0.1517 0.2452 0.5949 0.027 Uiso 1 1 calc R U . . .
C104 C -0.0420(2) 0.20248(15) 0.60810(11) 0.0273(7) Uani 1 1 d . . . . .
H104 H -0.0532 0.1971 0.6425 0.033 Uiso 1 1 calc R U . . .
C105 C 0.0366(2) 0.18079(14) 0.58722(11) 0.0248(7) Uani 1 1 d . . . . .
H105 H 0.0772 0.1609 0.6076 0.030 Uiso 1 1 calc R U . . .
C106 C 0.05337(18) 0.18868(13) 0.53770(11) 0.0180(6) Uani 1 1 d . . . . .
C107 C 0.13844(19) 0.16733(12) 0.51898(11) 0.0184(6) Uani 1 1 d . . . . .
C108 C 0.15319(18) 0.16963(12) 0.46496(11) 0.0175(6) Uani 1 1 d . . . . .
C109 C 0.22906(19) 0.14580(13) 0.44451(12) 0.0233(7) Uani 1 1 d . . . . .
H109 H 0.2706 0.1279 0.4657 0.028 Uiso 1 1 calc R U . . .
C110 C 0.24373(19) 0.14818(14) 0.39393(12) 0.0249(7) Uani 1 1 d . . . . .
H110 H 0.2951 0.1320 0.3804 0.030 Uiso 1 1 calc R U . . .
C111 C 0.18287(19) 0.17452(14) 0.36266(12) 0.0239(7) Uani 1 1 d . . . . .
H111 H 0.1933 0.1766 0.3279 0.029 Uiso 1 1 calc R U . . .
C112 C 0.10744(18) 0.19766(13) 0.38207(11) 0.0189(6) Uani 1 1 d . . . . .
H112 H 0.0663 0.2153 0.3605 0.023 Uiso 1 1 calc R U . . .
C113 C 0.09120(18) 0.19537(12) 0.43330(11) 0.0160(6) Uani 1 1 d . . . . .
C114 C 0.00917(17) 0.22013(12) 0.45361(10) 0.0138(5) Uani 1 1 d . . . . .
C115 C -0.00847(17) 0.21652(12) 0.50483(10) 0.0149(5) Uani 1 1 d . . . . .
O116 O -0.04129(12) 0.24254(8) 0.42041(7) 0.0142(4) Uani 1 1 d . . . . .
O117 O 0.19532(14) 0.14819(9) 0.54759(8) 0.0251(5) Uani 1 1 d . . . . .
C121 C -0.26591(17) 0.32194(11) 0.43558(10) 0.0139(5) Uani 1 1 d . . . . .
O122 O -0.33022(13) 0.34646(9) 0.44169(8) 0.0205(4) Uani 1 1 d . . . . .
P130 P -0.08970(5) 0.37169(3) 0.44361(3) 0.01405(14) Uani 1 1 d . . . . .
C131 C -0.14705(18) 0.43358(12) 0.41991(12) 0.0191(6) Uani 1 1 d . . . . .
C132 C -0.1973(2) 0.43150(14) 0.37634(12) 0.0310(8) Uani 1 1 d . . . . .
H132 H -0.2014 0.3976 0.3583 0.037 Uiso 1 1 calc R U . . .
C133 C -0.2416(3) 0.47828(15) 0.35878(15) 0.0393(9) Uani 1 1 d . . . . .
H133 H -0.2752 0.4762 0.3289 0.047 Uiso 1 1 calc R U . . .
C134 C -0.2368(2) 0.52719(15) 0.38453(15) 0.0379(9) Uani 1 1 d . . . . .
H134 H -0.2668 0.5591 0.3724 0.045 Uiso 1 1 calc R U . . .
C135 C -0.1888(3) 0.53018(16) 0.42772(17) 0.0492(12) Uani 1 1 d . . . . .
H135 H -0.1870 0.5638 0.4462 0.059 Uiso 1 1 calc R U . . .
C136 C -0.1426(2) 0.48405(15) 0.44465(16) 0.0414(10) Uani 1 1 d . . . . .
H136 H -0.1071 0.4872 0.4738 0.050 Uiso 1 1 calc R U . . .
C141 C -0.0870(2) 0.38717(12) 0.51020(11) 0.0200(6) Uani 1 1 d . . . . .
C142 C -0.1668(2) 0.39923(17) 0.53270(13) 0.0372(9) Uani 1 1 d . . . . .
H142 H -0.2194 0.3979 0.5134 0.045 Uiso 1 1 calc R U . . .
C143 C -0.1709(2) 0.41309(16) 0.58257(13) 0.0363(9) Uani 1 1 d . . . . .
H143 H -0.2258 0.4221 0.5970 0.044 Uiso 1 1 calc R U . . .
C144 C -0.0962(3) 0.41394(14) 0.61125(12) 0.0315(8) Uani 1 1 d . . . . .
H144 H -0.0992 0.4240 0.6454 0.038 Uiso 1 1 calc R U . . .
C145 C -0.0161(3) 0.40025(16) 0.59065(13) 0.0385(9) Uani 1 1 d . . . . .
H145 H 0.0357 0.4005 0.6106 0.046 Uiso 1 1 calc R U . . .
C146 C -0.0120(2) 0.38590(14) 0.53951(12) 0.0299(8) Uani 1 1 d . . . . .
H146 H 0.0424 0.3754 0.5254 0.036 Uiso 1 1 calc R U . . .
C151 C 0.02371(17) 0.38229(12) 0.42313(10) 0.0150(5) Uani 1 1 d . . . . .
C152 C 0.0718(2) 0.42869(14) 0.43775(13) 0.0276(7) Uani 1 1 d . . . . .
H152 H 0.0453 0.4560 0.4583 0.033 Uiso 1 1 calc R U . . .
C153 C 0.1582(2) 0.43567(15) 0.42266(14) 0.0334(8) Uani 1 1 d . . . . .
H153 H 0.1907 0.4672 0.4335 0.040 Uiso 1 1 calc R U . . .
C154 C 0.1970(2) 0.39670(14) 0.39187(12) 0.0236(7) Uani 1 1 d . . . . .
H154 H 0.2560 0.4014 0.3816 0.028 Uiso 1 1 calc R U . . .
C155 C 0.1495(2) 0.35118(14) 0.37621(12) 0.0264(7) Uani 1 1 d . . . . .
H155 H 0.1756 0.3246 0.3549 0.032 Uiso 1 1 calc R U . . .
C156 C 0.0630(2) 0.34411(13) 0.39169(12) 0.0235(7) Uani 1 1 d . . . . .
H156 H 0.0306 0.3127 0.3805 0.028 Uiso 1 1 calc R U . . .
P160 P -0.23626(4) 0.19674(3) 0.41633(3) 0.01136(13) Uani 1 1 d . . . . .
C161 C -0.35238(17) 0.20372(12) 0.39887(10) 0.0141(5) Uani 1 1 d . . . . .
C162 C -0.41574(19) 0.16462(13) 0.41330(11) 0.0194(6) Uani 1 1 d . . . . .
H162 H -0.3985 0.1336 0.4329 0.023 Uiso 1 1 calc R U . . .
C163 C -0.50321(19) 0.17077(13) 0.39920(11) 0.0212(6) Uani 1 1 d . . . . .
H163 H -0.5451 0.1438 0.4091 0.025 Uiso 1 1 calc R U . . .
C164 C -0.53002(19) 0.21616(13) 0.37066(11) 0.0212(6) Uani 1 1 d . . . . .
H164 H -0.5900 0.2206 0.3615 0.025 Uiso 1 1 calc R U . . .
C165 C -0.46793(19) 0.25491(13) 0.35578(10) 0.0188(6) Uani 1 1 d . . . . .
H165 H -0.4856 0.2859 0.3362 0.023 Uiso 1 1 calc R U . . .
C166 C -0.37963(18) 0.24874(12) 0.36941(10) 0.0155(6) Uani 1 1 d . . . . .
H166 H -0.3378 0.2753 0.3586 0.019 Uiso 1 1 calc R U . . .
C171 C -0.24017(17) 0.15621(12) 0.47382(10) 0.0139(5) Uani 1 1 d . . . . .
C172 C -0.29746(19) 0.17280(12) 0.51145(11) 0.0183(6) Uani 1 1 d . . . . .
H172 H -0.3356 0.2035 0.5059 0.022 Uiso 1 1 calc R U . . .
C173 C -0.2992(2) 0.14514(14) 0.55652(11) 0.0253(7) Uani 1 1 d . . . . .
H173 H -0.3385 0.1568 0.5817 0.030 Uiso 1 1 calc R U . . .
C174 C -0.2441(2) 0.10053(15) 0.56509(12) 0.0325(8) Uani 1 1 d . . . . .
H174 H -0.2466 0.0809 0.5957 0.039 Uiso 1 1 calc R U . . .
C175 C -0.1849(3) 0.08449(16) 0.52885(13) 0.0377(9) Uani 1 1 d . . . . .
H175 H -0.1456 0.0546 0.5352 0.045 Uiso 1 1 calc R U . . .
C176 C -0.1829(2) 0.11204(14) 0.48322(11) 0.0244(7) Uani 1 1 d . . . . .
H176 H -0.1425 0.1008 0.4585 0.029 Uiso 1 1 calc R U . . .
C181 C -0.19519(18) 0.14605(12) 0.37121(10) 0.0144(5) Uani 1 1 d . . . . .
C182 C -0.2416(2) 0.09737(13) 0.36151(12) 0.0239(7) Uani 1 1 d . . . . .
H182 H -0.2963 0.0913 0.3773 0.029 Uiso 1 1 calc R U . . .
C183 C -0.2092(2) 0.05747(14) 0.32899(13) 0.0284(8) Uani 1 1 d . . . . .
H183 H -0.2416 0.0245 0.3227 0.034 Uiso 1 1 calc R U . . .
C184 C -0.1293(2) 0.06602(13) 0.30573(11) 0.0239(7) Uani 1 1 d . . . . .
H184 H -0.1067 0.0387 0.2838 0.029 Uiso 1 1 calc R U . . .
C185 C -0.0830(2) 0.11437(13) 0.31455(11) 0.0224(7) Uani 1 1 d . . . . .
H185 H -0.0288 0.1204 0.2983 0.027 Uiso 1 1 calc R U . . .
C186 C -0.11526(18) 0.15440(13) 0.34704(10) 0.0181(6) Uani 1 1 d . . . . .
H186 H -0.0829 0.1875 0.3528 0.022 Uiso 1 1 calc R U . . .
C201 C 0.4396(2) 0.46366(15) 0.42328(13) 0.0351(8) Uani 1 1 d D . . . .
C202 C 0.4638(3) 0.50850(17) 0.39390(14) 0.0456(10) Uani 1 1 d D . . . .
H202 H 0.4920 0.5019 0.3631 0.055 Uiso 1 1 calc R U . . .
C203 C 0.4477(3) 0.56301(16) 0.40875(15) 0.0451(10) Uani 1 1 d D . . . .
H203 H 0.4647 0.5930 0.3880 0.054 Uiso 1 1 calc R U . . .
C204 C 0.4071(2) 0.57343(15) 0.45333(15) 0.0395(9) Uani 1 1 d D . . . .
H204 H 0.3959 0.6105 0.4634 0.047 Uiso 1 1 calc R U . . .
C205 C 0.3829(2) 0.52939(15) 0.48336(15) 0.0385(9) Uani 1 1 d D . . . .
H205 H 0.3557 0.5362 0.5145 0.046 Uiso 1 1 calc R U . . .
C206 C 0.3982(2) 0.47574(15) 0.46797(13) 0.0351(8) Uani 1 1 d D . . . .
H206 H 0.3800 0.4459 0.4886 0.042 Uiso 1 1 calc R U . . .
C207 C 0.4585(3) 0.40453(18) 0.40845(18) 0.0538(12) Uani 1 1 d D . . . .
H20A H 0.4252 0.3953 0.3782 0.081 Uiso 1 1 calc R U . . .
H20B H 0.4413 0.3795 0.4354 0.081 Uiso 1 1 calc R U . . .
H20C H 0.5214 0.4003 0.4022 0.081 Uiso 1 1 calc R U . . .
C301 C -0.0742(6) 0.4388(3) 0.1942(2) 0.061(2) Uani 0.399(4) 1 d DG U P A 2
H301 H -0.0855 0.4218 0.1628 0.073 Uiso 0.399(4) 1 calc R U P A 2
C302 C -0.0356(6) 0.4083(3) 0.2325(3) 0.083(3) Uani 0.399(4) 1 d DG U P A 2
H302 H -0.0205 0.3705 0.2273 0.100 Uiso 0.399(4) 1 calc R U P A 2
C303 C -0.0190(6) 0.4332(4) 0.2783(3) 0.063(2) Uani 0.399(4) 1 d DG U P A 2
H303 H 0.0074 0.4123 0.3045 0.076 Uiso 0.399(4) 1 calc R U P A 2
C304 C -0.0411(6) 0.4886(4) 0.2859(3) 0.0550(19) Uani 0.399(4) 1 d DG U P A 2
H304 H -0.0298 0.5056 0.3172 0.066 Uiso 0.399(4) 1 calc R U P A 2
C305 C -0.0797(7) 0.5191(3) 0.2476(3) 0.0490(16) Uani 0.399(4) 1 d DG U P A 2
H305 H -0.0948 0.5569 0.2527 0.059 Uiso 0.399(4) 1 calc R U P A 2
C306 C -0.0963(7) 0.4942(3) 0.2017(3) 0.0521(15) Uani 0.399(4) 1 d DG U P A 2
H306 H -0.1226 0.5151 0.1755 0.063 Uiso 0.399(4) 1 calc R U P A 2
C307 C -0.0995(15) 0.4107(8) 0.1466(5) 0.072(6) Uani 0.199(2) 1 d D U P A 2
H30A H -0.1249 0.4380 0.1236 0.108 Uiso 0.199(2) 1 calc R U P A 2
H30B H -0.1427 0.3816 0.1533 0.108 Uiso 0.199(2) 1 calc R U P A 2
H30C H -0.0473 0.3941 0.1316 0.108 Uiso 0.199(2) 1 calc R U P A 2
C308 C -0.1368(10) 0.5277(7) 0.1604(5) 0.066(6) Uani 0.301(2) 1 d D U P A 2
H30D H -0.1442 0.5043 0.1308 0.099 Uiso 0.301(2) 1 calc R U P A 2
H30E H -0.0986 0.5592 0.1525 0.099 Uiso 0.301(2) 1 calc R U P A 2
H30F H -0.1942 0.5416 0.1708 0.099 Uiso 0.301(2) 1 calc R U P A 2
C311 C -0.0578(4) 0.43639(18) 0.2317(2) 0.061(2) Uani 0.601(4) 1 d DG U P A 1
H311 H -0.0618 0.4032 0.2126 0.073 Uiso 0.601(4) 1 calc R U P A 1
C312 C -0.0196(4) 0.4353(2) 0.2789(2) 0.083(3) Uani 0.601(4) 1 d G U P A 1
H312 H 0.0025 0.4014 0.2921 0.100 Uiso 0.601(4) 1 calc R U P A 1
C313 C -0.0138(4) 0.4838(3) 0.30677(17) 0.063(2) Uani 0.601(4) 1 d G U P A 1
H313 H 0.0124 0.4831 0.3390 0.076 Uiso 0.601(4) 1 calc R U P A 1
C314 C -0.0461(4) 0.5334(2) 0.2874(2) 0.0550(19) Uani 0.601(4) 1 d G U P A 1
H314 H -0.0421 0.5666 0.3065 0.066 Uiso 0.601(4) 1 calc R U P A 1
C315 C -0.0843(4) 0.53449(18) 0.2402(2) 0.0490(16) Uani 0.601(4) 1 d G U P A 1
H315 H -0.1064 0.5684 0.2270 0.059 Uiso 0.601(4) 1 calc R U P A 1
C316 C -0.0901(4) 0.4860(2) 0.21235(17) 0.0521(15) Uani 0.601(4) 1 d DG U P A 1
H316 H -0.1162 0.4867 0.1801 0.063 Uiso 0.601(4) 1 calc R U P A 1
C317 C -0.0673(17) 0.3835(7) 0.2032(9) 0.072(6) Uani 0.199(2) 1 d D U P A 1
H31A H -0.0953 0.3911 0.1709 0.108 Uiso 0.199(2) 1 calc R U P A 1
H31B H -0.1037 0.3575 0.2220 0.108 Uiso 0.199(2) 1 calc R U P A 1
H31C H -0.0093 0.3671 0.1980 0.108 Uiso 0.199(2) 1 calc R U P A 1
C318 C -0.1346(11) 0.4867(10) 0.1628(4) 0.081(7) Uani 0.301(2) 1 d D U P A 1
H31D H -0.1332 0.4494 0.1482 0.122 Uiso 0.301(2) 1 calc R U P A 1
H31E H -0.1043 0.5128 0.1408 0.122 Uiso 0.301(2) 1 calc R U P A 1
H31F H -0.1957 0.4985 0.1667 0.122 Uiso 0.301(2) 1 calc R U P A 1
C401 C 0.0229(4) 0.0013(3) 0.5203(2) 0.042(2) Uani 0.5 1 d G U P . .
C402 C 0.0607(3) 0.0398(2) 0.4885(3) 0.052(3) Uani 0.5 1 d G U P . .
H402 H 0.1034 0.0652 0.5009 0.063 Uiso 0.5 1 calc R U P . .
C403 C 0.0360(4) 0.0412(2) 0.4385(2) 0.053(2) Uani 0.5 1 d G U P . .
H403 H 0.0618 0.0675 0.4168 0.063 Uiso 0.5 1 calc R U P . .
C404 C -0.0266(4) 0.0041(3) 0.4204(2) 0.047(3) Uani 0.5 1 d G U P . .
H404 H -0.0435 0.0051 0.3863 0.056 Uiso 0.5 1 calc R U P . .
C405 C -0.0643(3) -0.0344(2) 0.4523(3) 0.051(2) Uani 0.5 1 d G U P . .
H405 H -0.1071 -0.0597 0.4399 0.062 Uiso 0.5 1 calc R U P . .
C406 C -0.0396(3) -0.0358(2) 0.5022(2) 0.043(3) Uani 0.5 1 d G U P . .
H406 H -0.0654 -0.0621 0.5240 0.051 Uiso 0.5 1 calc R U P . .
C407 C 0.0509(9) 0.0006(5) 0.5734(5) 0.069(4) Uani 0.5 1 d . U P . .
H40A H 0.0190 -0.0287 0.5910 0.104 Uiso 0.5 1 calc R U P . .
H40B H 0.0381 0.0366 0.5886 0.104 Uiso 0.5 1 calc R U P . .
H40C H 0.1141 -0.0068 0.5757 0.104 Uiso 0.5 1 calc R U P . .


_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 C21 1.844(3) . ?
Os1 N1 2.037(2) . ?
Os1 O16 2.0940(19) . ?
Os1 P60 2.3830(8) . ?
Os1 P30 2.4084(8) . ?
Os1 Br1 2.5829(6) . ?
N1 C2 1.328(3) . ?
C2 C3 1.447(4) . ?
C2 C15 1.455(4) . ?
C3 C4 1.355(4) . ?
C4 C5 1.419(4) . ?
C5 C6 1.372(4) . ?
C6 C15 1.454(4) . ?
C6 C7 1.486(4) . ?
C7 O17 1.235(3) . ?
C7 C8 1.476(4) . ?
C8 C9 1.406(4) . ?
C8 C13 1.407(4) . ?
C9 C10 1.384(4) . ?
C10 C11 1.390(4) . ?
C11 C12 1.389(4) . ?
C12 C13 1.402(4) . ?
C13 C14 1.484(4) . ?
C14 O16 1.286(3) . ?
C14 C15 1.418(4) . ?
C21 O22 1.166(3) . ?
P30 C41 1.832(3) . ?
P30 C51 1.839(3) . ?
P30 C31 1.839(3) . ?
C31 C32 1.393(4) . ?
C31 C36 1.401(4) . ?
C32 C33 1.393(4) . ?
C33 C34 1.391(4) . ?
C34 C35 1.386(4) . ?
C35 C36 1.392(4) . ?
C41 C46 1.398(4) . ?
C41 C42 1.399(4) . ?
C42 C43 1.401(4) . ?
C43 C44 1.387(5) . ?
C44 C45 1.396(4) . ?
C45 C46 1.386(4) . ?
C51 C56 1.388(4) . ?
C51 C52 1.400(4) . ?
C52 C53 1.392(5) . ?
C53 C54 1.381(5) . ?
C54 C55 1.389(5) . ?
C55 C56 1.393(4) . ?
P60 C71 1.825(3) . ?
P60 C61 1.836(3) . ?
P60 C81 1.838(3) . ?
C61 C62 1.401(4) . ?
C61 C66 1.403(4) . ?
C62 C63 1.391(4) . ?
C63 C64 1.384(5) . ?
C64 C65 1.394(5) . ?
C65 C66 1.388(4) . ?
C71 C72 1.396(4) . ?
C71 C76 1.403(4) . ?
C72 C73 1.395(4) . ?
C73 C74 1.388(5) . ?
C74 C75 1.373(5) . ?
C75 C76 1.400(4) . ?
C81 C86 1.391(4) . ?
C81 C82 1.399(4) . ?
C82 C83 1.389(4) . ?
C83 C84 1.392(5) . ?
C84 C85 1.374(5) . ?
C85 C86 1.391(4) . ?
Os2 C121 1.849(3) . ?
Os2 N101 2.034(2) . ?
Os2 O116 2.0968(18) . ?
Os2 P130 2.4034(8) . ?
Os2 P160 2.4172(8) . ?
Os2 Br2 2.5755(6) . ?
N101 C102 1.319(4) . ?
C102 C103 1.453(4) . ?
C102 C115 1.457(4) . ?
C103 C104 1.348(4) . ?
C104 C105 1.427(4) . ?
C105 C106 1.370(4) . ?
C106 C115 1.449(4) . ?
C106 C107 1.487(4) . ?
C107 O117 1.241(3) . ?
C107 C108 1.472(4) . ?
C108 C109 1.407(4) . ?
C108 C113 1.408(4) . ?
C109 C110 1.380(4) . ?
C110 C111 1.397(4) . ?
C111 C112 1.384(4) . ?
C112 C113 1.402(4) . ?
C113 C114 1.493(4) . ?
C114 O116 1.290(3) . ?
C114 C115 1.407(4) . ?
C121 O122 1.157(3) . ?
P130 C141 1.827(3) . ?
P130 C151 1.837(3) . ?
P130 C131 1.838(3) . ?
C131 C136 1.386(4) . ?
C131 C132 1.393(5) . ?
C132 C133 1.393(5) . ?
C133 C134 1.367(5) . ?
C134 C135 1.367(5) . ?
C135 C136 1.389(5) . ?
C141 C146 1.381(5) . ?
C141 C142 1.395(4) . ?
C142 C143 1.382(5) . ?
C143 C144 1.369(5) . ?
C144 C145 1.384(5) . ?
C145 C146 1.418(5) . ?
C151 C156 1.388(4) . ?
C151 C152 1.390(4) . ?
C152 C153 1.393(4) . ?
C153 C154 1.387(5) . ?
C154 C155 1.376(4) . ?
C155 C156 1.397(4) . ?
P160 C171 1.828(3) . ?
P160 C161 1.834(3) . ?
P160 C181 1.834(3) . ?
C161 C166 1.402(4) . ?
C161 C162 1.406(4) . ?
C162 C163 1.390(4) . ?
C163 C164 1.393(4) . ?
C164 C165 1.390(4) . ?
C165 C166 1.399(4) . ?
C171 C176 1.397(4) . ?
C171 C172 1.401(4) . ?
C172 C173 1.382(4) . ?
C173 C174 1.382(5) . ?
C174 C175 1.389(5) . ?
C175 C176 1.394(4) . ?
C181 C182 1.392(4) . ?
C181 C186 1.401(4) . ?
C182 C183 1.392(4) . ?
C183 C184 1.389(4) . ?
C184 C185 1.380(4) . ?
C185 C186 1.393(4) . ?
C201 C202 1.389(5) . ?
C201 C206 1.392(4) . ?
C201 C207 1.507(5) . ?
C202 C203 1.394(5) . ?
C203 C204 1.376(5) . ?
C204 C205 1.385(5) . ?
C205 C206 1.377(5) . ?
C301 C302 1.3900 . ?
C301 C306 1.3900 . ?
C301 C307 1.493(8) . ?
C302 C303 1.3900 . ?
C303 C304 1.3900 . ?
C304 C305 1.3900 . ?
C305 C306 1.3900 . ?
C306 C308 1.501(8) . ?
C311 C312 1.3900 . ?
C311 C316 1.3900 . ?
C311 C317 1.491(9) . ?
C312 C313 1.3900 . ?
C313 C314 1.3900 . ?
C314 C315 1.3900 . ?
C315 C316 1.3900 . ?
C316 C318 1.488(8) . ?
C401 C402 1.3900 . ?
C401 C406 1.3900 . ?
C401 C407 1.484(13) . ?
C402 C403 1.3900 . ?
C403 C404 1.3900 . ?
C404 C405 1.3900 . ?
C405 C406 1.3900 . ?

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
C21 Os1 N1 93.83(10) . . ?
C21 Os1 O16 178.87(10) . . ?
N1 Os1 O16 86.57(8) . . ?
C21 Os1 P60 90.18(9) . . ?
N1 Os1 P60 91.35(7) . . ?
O16 Os1 P60 88.76(6) . . ?
C21 Os1 P30 91.05(9) . . ?
N1 Os1 P30 88.48(7) . . ?
O16 Os1 P30 90.02(6) . . ?
P60 Os1 P30 178.78(2) . . ?
C21 Os1 Br1 95.94(8) . . ?
N1 Os1 Br1 170.21(6) . . ?
O16 Os1 Br1 83.68(5) . . ?
P60 Os1 Br1 89.301(18) . . ?
P30 Os1 Br1 90.658(18) . . ?
C2 N1 Os1 129.74(19) . . ?
N1 C2 C3 117.6(2) . . ?
N1 C2 C15 124.7(2) . . ?
C3 C2 C15 117.7(2) . . ?
C4 C3 C2 122.3(3) . . ?
C3 C4 C5 120.2(3) . . ?
C6 C5 C4 120.7(2) . . ?
C5 C6 C15 121.3(3) . . ?
C5 C6 C7 117.6(2) . . ?
C15 C6 C7 121.2(2) . . ?
O17 C7 C8 121.0(3) . . ?
O17 C7 C6 121.6(3) . . ?
C8 C7 C6 117.4(2) . . ?
C9 C8 C13 119.9(3) . . ?
C9 C8 C7 119.8(2) . . ?
C13 C8 C7 120.3(2) . . ?
C10 C9 C8 120.4(3) . . ?
C9 C10 C11 119.8(3) . . ?
C12 C11 C10 120.3(3) . . ?
C11 C12 C13 120.8(3) . . ?
C12 C13 C8 118.7(3) . . ?
C12 C13 C14 120.0(2) . . ?
C8 C13 C14 121.3(2) . . ?
O16 C14 C15 125.6(2) . . ?
O16 C14 C13 114.4(2) . . ?
C15 C14 C13 120.0(2) . . ?
C14 C15 C6 119.3(2) . . ?
C14 C15 C2 123.2(2) . . ?
C6 C15 C2 117.5(2) . . ?
C14 O16 Os1 129.83(17) . . ?
O22 C21 Os1 178.0(3) . . ?
C41 P30 C51 101.61(13) . . ?
C41 P30 C31 105.15(13) . . ?
C51 P30 C31 102.42(13) . . ?
C41 P30 Os1 111.80(9) . . ?
C51 P30 Os1 120.77(10) . . ?
C31 P30 Os1 113.36(10) . . ?
C32 C31 C36 119.1(3) . . ?
C32 C31 P30 123.4(2) . . ?
C36 C31 P30 117.5(2) . . ?
C33 C32 C31 120.7(3) . . ?
C34 C33 C32 120.0(3) . . ?
C35 C34 C33 119.6(3) . . ?
C34 C35 C36 120.8(3) . . ?
C35 C36 C31 119.9(3) . . ?
C46 C41 C42 118.8(3) . . ?
C46 C41 P30 121.2(2) . . ?
C42 C41 P30 119.5(2) . . ?
C41 C42 C43 120.4(3) . . ?
C44 C43 C42 120.2(3) . . ?
C43 C44 C45 119.5(3) . . ?
C46 C45 C44 120.3(3) . . ?
C45 C46 C41 120.8(3) . . ?
C56 C51 C52 118.6(3) . . ?
C56 C51 P30 122.4(2) . . ?
C52 C51 P30 118.9(2) . . ?
C53 C52 C51 120.8(3) . . ?
C54 C53 C52 119.8(3) . . ?
C53 C54 C55 120.2(3) . . ?
C54 C55 C56 119.9(3) . . ?
C51 C56 C55 120.7(3) . . ?
C71 P60 C61 106.29(13) . . ?
C71 P60 C81 103.53(13) . . ?
C61 P60 C81 100.95(13) . . ?
C71 P60 Os1 110.74(10) . . ?
C61 P60 Os1 115.87(10) . . ?
C81 P60 Os1 118.06(10) . . ?
C62 C61 C66 117.8(3) . . ?
C62 C61 P60 118.2(2) . . ?
C66 C61 P60 123.9(2) . . ?
C63 C62 C61 121.2(3) . . ?
C64 C63 C62 120.4(3) . . ?
C63 C64 C65 119.3(3) . . ?
C66 C65 C64 120.5(3) . . ?
C65 C66 C61 120.9(3) . . ?
C72 C71 C76 118.8(3) . . ?
C72 C71 P60 121.8(2) . . ?
C76 C71 P60 118.6(2) . . ?
C73 C72 C71 120.5(3) . . ?
C74 C73 C72 120.1(3) . . ?
C75 C74 C73 120.0(3) . . ?
C74 C75 C76 120.7(3) . . ?
C75 C76 C71 119.9(3) . . ?
C86 C81 C82 118.9(3) . . ?
C86 C81 P60 122.7(2) . . ?
C82 C81 P60 118.4(2) . . ?
C83 C82 C81 120.8(3) . . ?
C82 C83 C84 119.4(3) . . ?
C85 C84 C83 120.2(3) . . ?
C84 C85 C86 120.7(3) . . ?
C85 C86 C81 120.0(3) . . ?
C121 Os2 N101 93.93(10) . . ?
C121 Os2 O116 179.15(10) . . ?
N101 Os2 O116 86.00(8) . . ?
C121 Os2 P130 86.68(9) . . ?
N101 Os2 P130 89.07(7) . . ?
O116 Os2 P130 92.48(6) . . ?
C121 Os2 P160 91.92(9) . . ?
N101 Os2 P160 89.01(7) . . ?
O116 Os2 P160 88.92(6) . . ?
P130 Os2 P160 177.55(2) . . ?
C121 Os2 Br2 95.07(8) . . ?
N101 Os2 Br2 170.89(7) . . ?
O116 Os2 Br2 85.03(5) . . ?
P130 Os2 Br2 92.909(19) . . ?
P160 Os2 Br2 89.220(18) . . ?
C102 N101 Os2 130.53(19) . . ?
N101 C102 C103 117.5(3) . . ?
N101 C102 C115 124.9(2) . . ?
C103 C102 C115 117.6(3) . . ?
C104 C103 C102 122.0(3) . . ?
C103 C104 C105 121.0(3) . . ?
C106 C105 C104 119.8(3) . . ?
C105 C106 C115 121.9(3) . . ?
C105 C106 C107 116.9(3) . . ?
C115 C106 C107 121.2(3) . . ?
O117 C107 C108 120.8(3) . . ?
O117 C107 C106 121.6(3) . . ?
C108 C107 C106 117.6(2) . . ?
C109 C108 C113 119.5(3) . . ?
C109 C108 C107 120.3(3) . . ?
C113 C108 C107 120.2(3) . . ?
C110 C109 C108 120.6(3) . . ?
C109 C110 C111 119.8(3) . . ?
C112 C111 C110 120.3(3) . . ?
C111 C112 C113 120.6(3) . . ?
C112 C113 C108 119.1(3) . . ?
C112 C113 C114 120.0(3) . . ?
C108 C113 C114 120.9(3) . . ?
O116 C114 C115 125.7(2) . . ?
O116 C114 C113 114.2(2) . . ?
C115 C114 C113 120.1(2) . . ?
C114 C115 C106 119.6(2) . . ?
C114 C115 C102 122.8(2) . . ?
C106 C115 C102 117.6(2) . . ?
C114 O116 Os2 130.07(17) . . ?
O122 C121 Os2 177.5(3) . . ?
C141 P130 C151 104.65(13) . . ?
C141 P130 C131 100.34(14) . . ?
C151 P130 C131 103.24(13) . . ?
C141 P130 Os2 110.57(10) . . ?
C151 P130 Os2 119.77(10) . . ?
C131 P130 Os2 115.99(10) . . ?
C136 C131 C132 117.3(3) . . ?
C136 C131 P130 121.6(3) . . ?
C132 C131 P130 121.1(2) . . ?
C131 C132 C133 121.1(3) . . ?
C134 C133 C132 120.1(4) . . ?
C135 C134 C133 120.0(3) . . ?
C134 C135 C136 120.0(4) . . ?
C131 C136 C135 121.4(4) . . ?
C146 C141 C142 118.6(3) . . ?
C146 C141 P130 124.3(2) . . ?
C142 C141 P130 117.1(2) . . ?
C143 C142 C141 121.2(3) . . ?
C144 C143 C142 120.2(3) . . ?
C143 C144 C145 120.2(3) . . ?
C144 C145 C146 119.5(4) . . ?
C141 C146 C145 120.1(3) . . ?
C156 C151 C152 118.3(3) . . ?
C156 C151 P130 120.2(2) . . ?
C152 C151 P130 121.4(2) . . ?
C151 C152 C153 120.8(3) . . ?
C154 C153 C152 120.1(3) . . ?
C155 C154 C153 119.7(3) . . ?
C154 C155 C156 120.0(3) . . ?
C151 C156 C155 121.0(3) . . ?
C171 P160 C161 103.00(12) . . ?
C171 P160 C181 102.54(13) . . ?
C161 P160 C181 103.12(13) . . ?
C171 P160 Os2 111.83(9) . . ?
C161 P160 Os2 114.13(9) . . ?
C181 P160 Os2 120.23(9) . . ?
C166 C161 C162 118.2(3) . . ?
C166 C161 P160 119.6(2) . . ?
C162 C161 P160 122.1(2) . . ?
C163 C162 C161 120.9(3) . . ?
C162 C163 C164 120.6(3) . . ?
C165 C164 C163 119.2(3) . . ?
C164 C165 C166 120.6(3) . . ?
C165 C166 C161 120.5(3) . . ?
C176 C171 C172 118.7(3) . . ?
C176 C171 P160 122.2(2) . . ?
C172 C171 P160 118.9(2) . . ?
C173 C172 C171 120.8(3) . . ?
C174 C173 C172 120.2(3) . . ?
C173 C174 C175 119.9(3) . . ?
C174 C175 C176 120.3(3) . . ?
C175 C176 C171 120.1(3) . . ?
C182 C181 C186 118.5(3) . . ?
C182 C181 P160 120.5(2) . . ?
C186 C181 P160 121.0(2) . . ?
C183 C182 C181 121.0(3) . . ?
C184 C183 C182 119.9(3) . . ?
C185 C184 C183 119.8(3) . . ?
C184 C185 C186 120.5(3) . . ?
C185 C186 C181 120.3(3) . . ?
C202 C201 C206 116.9(3) . . ?
C202 C201 C207 122.1(3) . . ?
C206 C201 C207 121.0(3) . . ?
C201 C202 C203 121.3(3) . . ?
C204 C203 C202 120.2(3) . . ?
C203 C204 C205 119.5(3) . . ?
C206 C205 C204 119.7(3) . . ?
C205 C206 C201 122.3(3) . . ?
C302 C301 C306 120.0 . . ?
C302 C301 C307 119.9(8) . . ?
C306 C301 C307 119.9(8) . . ?
C301 C302 C303 120.0 . . ?
C304 C303 C302 120.0 . . ?
C303 C304 C305 120.0 . . ?
C304 C305 C306 120.0 . . ?
C305 C306 C301 120.0 . . ?
C305 C306 C308 119.6(9) . . ?
C301 C306 C308 120.4(9) . . ?
C312 C311 C316 120.0 . . ?
C312 C311 C317 119.3(11) . . ?
C316 C311 C317 120.6(11) . . ?
C313 C312 C311 120.0 . . ?
C312 C313 C314 120.0 . . ?
C315 C314 C313 120.0 . . ?
C316 C315 C314 120.0 . . ?
C315 C316 C311 120.0 . . ?
C315 C316 C318 119.8(10) . . ?
C311 C316 C318 120.1(10) . . ?
C402 C401 C406 120.0 . . ?
C402 C401 C407 118.8(7) . . ?
C406 C401 C407 121.2(6) . . ?
C403 C402 C401 120.0 . . ?
C402 C403 C404 120.0 . . ?
C405 C404 C403 120.0 . . ?
C406 C405 C404 120.0 . . ?
C405 C406 C401 120.0 . . ?

_refine_diff_density_max         1.655
_refine_diff_density_min         -1.234
_refine_diff_density_rms         0.139

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_8619
_database_code_depnum_ccdc_archive 'CCDC 1447863'
_audit_update_record             
;
2016-07-02 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_audit_creation_date             2014-01-20
_audit_block_code                FNG-PG-511-06
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_compound_source        'dichloromethane, hexane'
_chemical_formula_moiety         'C51 H38 Cl N O3 P2 Ru'
_chemical_formula_sum            'C51 H38 Cl N O3 P2 Ru'
_chemical_formula_weight         911.28

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'
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'
Ru Ru -1.2594 0.8363 '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                   9.475(2)
_cell_length_b                   17.056(2)
_cell_length_c                   25.674(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.548(13)
_cell_angle_gamma                90
_cell_volume                     4103.0(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    102431
_cell_measurement_theta_min      2.6862
_cell_measurement_theta_max      34.9999

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 1.00 0.0700
1.00 0.00 -1.00 0.0700
0.00 0.00 1.00 0.0800
0.00 0.00 -1.00 0.0800
0.00 1.00 0.00 0.0450
0.00 -1.00 0.00 0.0450
0.00 1.00 -1.00 0.0450
0.00 -1.00 -1.00 0.0550
-1.00 0.00 -2.00 0.0900

_exptl_crystal_description       Prism
_exptl_crystal_colour            darkgreen
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    0.572
_shelx_estimated_absorpt_T_min   0.914
_shelx_estimated_absorpt_T_max   0.950
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_absorpt_correction_T_min  0.92314
_exptl_absorpt_correction_T_max  0.95519

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_detector_area_resol_mean 18.02
_diffrn_reflns_number            95037
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.687
_diffrn_reflns_theta_max         34.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             18036
_reflns_number_gt                16336
_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       'DATCOL (Bruker AXS, 2006)'
_computing_cell_refinement       'DENZO (Bruker AXS, 2006)'
_computing_data_reduction        'DENZO (Bruker AXS, 2006)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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+3.1303P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18036
_refine_ls_number_parameters     535
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0833
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.003
_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
Ru1 Ru -0.63499(2) 0.31400(2) 0.59624(2) 0.01088(2) Uani 1 1 d . . . . .
Cl20 Cl -0.89175(3) 0.31838(2) 0.59310(2) 0.01589(5) Uani 1 1 d . . . . .
N1 N -0.41918(10) 0.30398(6) 0.61144(4) 0.01389(15) Uani 1 1 d D . . . .
H1 H -0.3679(19) 0.3106(10) 0.5859(7) 0.017 Uiso 1 1 d D U . . .
C2 C -0.33604(12) 0.29468(6) 0.65718(4) 0.01387(17) Uani 1 1 d . . . . .
C3 C -0.18350(12) 0.29577(7) 0.65777(5) 0.01816(19) Uani 1 1 d . . . . .
H3 H -0.1472 0.2979 0.6252 0.022 Uiso 1 1 calc R U . . .
C4 C -0.09005(13) 0.29392(8) 0.70349(6) 0.0215(2) Uani 1 1 d . . . . .
H4 H 0.0097 0.2955 0.7024 0.026 Uiso 1 1 calc R U . . .
C5 C -0.14002(13) 0.28963(8) 0.75271(5) 0.0202(2) Uani 1 1 d . . . . .
H5 H -0.0743 0.2912 0.7845 0.024 Uiso 1 1 calc R U . . .
C6 C -0.28421(13) 0.28323(7) 0.75440(5) 0.01644(19) Uani 1 1 d . . . . .
C7 C -0.33029(14) 0.27534(7) 0.80710(5) 0.0185(2) Uani 1 1 d . . . . .
C8 C -0.48071(14) 0.25332(7) 0.80855(5) 0.01723(19) Uani 1 1 d . . . . .
C9 C -0.52693(16) 0.23899(8) 0.85697(5) 0.0235(2) Uani 1 1 d . . . . .
H9 H -0.4627 0.2455 0.8888 0.028 Uiso 1 1 calc R U . . .
C10 C -0.66638(17) 0.21521(9) 0.85869(5) 0.0256(3) Uani 1 1 d . . . . .
H10 H -0.6973 0.2055 0.8916 0.031 Uiso 1 1 calc R U . . .
C11 C -0.76100(15) 0.20565(8) 0.81198(5) 0.0227(2) Uani 1 1 d . . . . .
H11 H -0.8559 0.1887 0.8132 0.027 Uiso 1 1 calc R U . . .
C12 C -0.71697(13) 0.22089(7) 0.76372(5) 0.0182(2) Uani 1 1 d . . . . .
H12 H -0.7821 0.2147 0.7321 0.022 Uiso 1 1 calc R U . . .
C13 C -0.57634(13) 0.24540(7) 0.76156(4) 0.01498(18) Uani 1 1 d . . . . .
C14 C -0.53245(12) 0.26586(6) 0.71004(4) 0.01297(16) Uani 1 1 d . . . . .
C15 C -0.38718(12) 0.28268(6) 0.70702(4) 0.01352(17) Uani 1 1 d . . . . .
O16 O -0.63343(9) 0.26623(5) 0.67129(3) 0.01391(13) Uani 1 1 d . . . . .
O17 O -0.24689(12) 0.28605(7) 0.84787(4) 0.0272(2) Uani 1 1 d . . . . .
C31 C -0.64368(12) 0.35626(7) 0.53018(5) 0.01584(18) Uani 1 1 d . . . . .
O32 O -0.65182(12) 0.38353(6) 0.48885(4) 0.02414(19) Uani 1 1 d . . . . .
P40 P -0.61018(3) 0.44715(2) 0.62923(2) 0.01248(5) Uani 1 1 d . . . . .
C41 C -0.67699(13) 0.47355(7) 0.69017(4) 0.01532(18) Uani 1 1 d . . . . .
C42 C -0.65578(17) 0.54967(8) 0.71066(6) 0.0240(2) Uani 1 1 d . . . . .
H42 H -0.6090 0.5878 0.6924 0.029 Uiso 1 1 calc R U . . .
C43 C -0.70336(19) 0.56929(8) 0.75785(6) 0.0286(3) Uani 1 1 d . . . . .
H43 H -0.6885 0.6207 0.7718 0.034 Uiso 1 1 calc R U . . .
C44 C -0.77271(17) 0.51337(9) 0.78461(6) 0.0258(3) Uani 1 1 d . . . . .
H44 H -0.8033 0.5265 0.8171 0.031 Uiso 1 1 calc R U . . .
C45 C -0.79704(16) 0.43862(8) 0.76377(5) 0.0230(2) Uani 1 1 d . . . . .
H45 H -0.8458 0.4009 0.7817 0.028 Uiso 1 1 calc R U . . .
C46 C -0.74999(13) 0.41875(7) 0.71647(5) 0.01731(19) Uani 1 1 d . . . . .
H46 H -0.7678 0.3677 0.7021 0.021 Uiso 1 1 calc R U . . .
C51 C -0.42173(12) 0.47490(6) 0.63990(5) 0.01465(17) Uani 1 1 d . . . . .
C52 C -0.34447(13) 0.48872(7) 0.68959(5) 0.0185(2) Uani 1 1 d . . . . .
H52 H -0.3915 0.4888 0.7198 0.022 Uiso 1 1 calc R U . . .
C53 C -0.19703(14) 0.50245(9) 0.69485(5) 0.0231(2) Uani 1 1 d . . . . .
H53 H -0.1447 0.5120 0.7288 0.028 Uiso 1 1 calc R U . . .
C54 C -0.12671(14) 0.50222(8) 0.65127(6) 0.0233(2) Uani 1 1 d . . . . .
H54 H -0.0269 0.5118 0.6552 0.028 Uiso 1 1 calc R U . . .
C55 C -0.20333(14) 0.48791(8) 0.60160(5) 0.0209(2) Uani 1 1 d . . . . .
H55 H -0.1558 0.4877 0.5715 0.025 Uiso 1 1 calc R U . . .
C56 C -0.34925(13) 0.47387(7) 0.59599(5) 0.01729(19) Uani 1 1 d . . . . .
H56 H -0.4006 0.4634 0.5620 0.021 Uiso 1 1 calc R U . . .
C61 C -0.69421(12) 0.52264(6) 0.58390(4) 0.01474(17) Uani 1 1 d . . . . .
C62 C -0.84189(13) 0.51885(8) 0.56739(6) 0.0213(2) Uani 1 1 d . . . . .
H62 H -0.8954 0.4765 0.5785 0.026 Uiso 1 1 calc R U . . .
C63 C -0.91064(14) 0.57683(8) 0.53474(6) 0.0241(2) Uani 1 1 d . . . . .
H63 H -1.0111 0.5743 0.5244 0.029 Uiso 1 1 calc R U . . .
C64 C -0.83366(14) 0.63821(7) 0.51720(5) 0.0199(2) Uani 1 1 d . . . . .
H64 H -0.8808 0.6774 0.4947 0.024 Uiso 1 1 calc R U . . .
C65 C -0.68764(14) 0.64174(7) 0.53277(5) 0.0210(2) Uani 1 1 d . . . . .
H65 H -0.6343 0.6832 0.5204 0.025 Uiso 1 1 calc R U . . .
C66 C -0.61786(13) 0.58489(7) 0.56648(5) 0.0188(2) Uani 1 1 d . . . . .
H66 H -0.5179 0.5887 0.5776 0.023 Uiso 1 1 calc R U . . .
P70 P -0.64461(3) 0.18373(2) 0.56004(2) 0.01285(5) Uani 1 1 d . . . . .
C71 C -0.47240(13) 0.15547(6) 0.54160(5) 0.01551(18) Uani 1 1 d . . . . .
C72 C -0.44778(14) 0.15588(7) 0.48913(5) 0.0191(2) Uani 1 1 d . . . . .
H72 H -0.5250 0.1639 0.4615 0.023 Uiso 1 1 calc R U . . .
C73 C -0.31002(16) 0.14451(8) 0.47722(6) 0.0233(2) Uani 1 1 d . . . . .
H73 H -0.2942 0.1448 0.4415 0.028 Uiso 1 1 calc R U . . .
C74 C -0.19603(15) 0.13284(8) 0.51717(6) 0.0247(2) Uani 1 1 d . . . . .
H74 H -0.1025 0.1255 0.5089 0.030 Uiso 1 1 calc R U . . .
C75 C -0.21969(14) 0.13196(8) 0.56949(6) 0.0219(2) Uani 1 1 d . . . . .
H75 H -0.1420 0.1239 0.5969 0.026 Uiso 1 1 calc R U . . .
C76 C -0.35651(13) 0.14288(7) 0.58163(5) 0.01793(19) Uani 1 1 d . . . . .
H76 H -0.3718 0.1418 0.6174 0.022 Uiso 1 1 calc R U . . .
C81 C -0.68538(13) 0.10589(7) 0.60453(5) 0.01638(18) Uani 1 1 d . . . . .
C82 C -0.60965(16) 0.03526(7) 0.61128(5) 0.0224(2) Uani 1 1 d . . . . .
H82 H -0.5307 0.0267 0.5931 0.027 Uiso 1 1 calc R U . . .
C83 C -0.64967(18) -0.02262(8) 0.64463(6) 0.0261(3) Uani 1 1 d . . . . .
H83 H -0.5964 -0.0699 0.6499 0.031 Uiso 1 1 calc R U . . .
C84 C -0.76721(17) -0.01117(8) 0.67010(5) 0.0246(2) Uani 1 1 d . . . . .
H84 H -0.7955 -0.0509 0.6923 0.029 Uiso 1 1 calc R U . . .
C85 C -0.84383(15) 0.05870(9) 0.66306(6) 0.0241(2) Uani 1 1 d . . . . .
H85 H -0.9245 0.0663 0.6805 0.029 Uiso 1 1 calc R U . . .
C86 C -0.80307(14) 0.11751(8) 0.63072(5) 0.0200(2) Uani 1 1 d . . . . .
H86 H -0.8550 0.1653 0.6265 0.024 Uiso 1 1 calc R U . . .
C91 C -0.77238(13) 0.16429(7) 0.50080(4) 0.01589(18) Uani 1 1 d . . . . .
C92 C -0.78389(16) 0.08848(8) 0.47951(6) 0.0250(3) Uani 1 1 d . . . . .
H92 H -0.7265 0.0473 0.4962 0.030 Uiso 1 1 calc R U . . .
C93 C -0.87929(18) 0.07337(8) 0.43394(6) 0.0295(3) Uani 1 1 d . . . . .
H93 H -0.8863 0.0220 0.4195 0.035 Uiso 1 1 calc R U . . .
C94 C -0.96463(15) 0.13321(8) 0.40932(5) 0.0237(2) Uani 1 1 d . . . . .
H94 H -1.0289 0.1227 0.3780 0.028 Uiso 1 1 calc R U . . .
C95 C -0.95550(13) 0.20816(8) 0.43057(5) 0.0187(2) Uani 1 1 d . . . . .
H95 H -1.0142 0.2489 0.4140 0.022 Uiso 1 1 calc R U . . .
C96 C -0.85993(13) 0.22365(7) 0.47624(5) 0.01618(18) Uani 1 1 d . . . . .
H96 H -0.8543 0.2750 0.4908 0.019 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
Ru1 C31 1.8335(12) . ?
Ru1 N1 2.0311(11) . ?
Ru1 O16 2.0901(9) . ?
Ru1 P70 2.4049(4) . ?
Ru1 P40 2.4229(4) . ?
Ru1 Cl20 2.4233(6) . ?
N1 C2 1.3228(15) . ?
C2 C3 1.4432(16) . ?
C2 C15 1.4487(16) . ?
C3 C4 1.3616(18) . ?
C4 C5 1.416(2) . ?
C5 C6 1.3776(18) . ?
C6 C15 1.4418(16) . ?
C6 C7 1.4884(18) . ?
C7 O17 1.2279(15) . ?
C7 C8 1.4797(19) . ?
C8 C9 1.3994(18) . ?
C8 C13 1.4036(16) . ?
C9 C10 1.389(2) . ?
C10 C11 1.396(2) . ?
C11 C12 1.3895(17) . ?
C12 C13 1.4054(17) . ?
C13 C14 1.4859(16) . ?
C14 O16 1.2737(13) . ?
C14 C15 1.4193(16) . ?
C31 O32 1.1505(15) . ?
P40 C51 1.8282(12) . ?
P40 C41 1.8292(12) . ?
P40 C61 1.8360(11) . ?
C41 C46 1.3952(16) . ?
C41 C42 1.4041(17) . ?
C42 C43 1.3947(19) . ?
C43 C44 1.396(2) . ?
C44 C45 1.389(2) . ?
C45 C46 1.3961(17) . ?
C51 C52 1.3934(17) . ?
C51 C56 1.4047(16) . ?
C52 C53 1.4030(18) . ?
C53 C54 1.385(2) . ?
C54 C55 1.392(2) . ?
C55 C56 1.3894(18) . ?
C61 C66 1.3953(16) . ?
C61 C62 1.4020(17) . ?
C62 C63 1.3937(18) . ?
C63 C64 1.3888(19) . ?
C64 C65 1.3832(19) . ?
C65 C66 1.3988(17) . ?
P70 C91 1.8282(12) . ?
P70 C81 1.8295(12) . ?
P70 C71 1.8299(12) . ?
C71 C72 1.4009(17) . ?
C71 C76 1.4044(17) . ?
C72 C73 1.3977(19) . ?
C73 C74 1.389(2) . ?
C74 C75 1.394(2) . ?
C75 C76 1.3901(18) . ?
C81 C86 1.3992(18) . ?
C81 C82 1.3997(18) . ?
C82 C83 1.3957(19) . ?
C83 C84 1.387(2) . ?
C84 C85 1.393(2) . ?
C85 C86 1.3930(18) . ?
C91 C96 1.3983(16) . ?
C91 C92 1.4017(17) . ?
C92 C93 1.3921(19) . ?
C93 C94 1.394(2) . ?
C94 C95 1.3875(19) . ?
C95 C96 1.3961(17) . ?

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
C31 Ru1 N1 96.68(5) . . ?
C31 Ru1 O16 177.84(4) . . ?
N1 Ru1 O16 85.48(4) . . ?
C31 Ru1 P70 90.68(4) . . ?
N1 Ru1 P70 88.61(3) . . ?
O16 Ru1 P70 89.47(3) . . ?
C31 Ru1 P40 86.77(4) . . ?
N1 Ru1 P40 88.23(3) . . ?
O16 Ru1 P40 93.22(3) . . ?
P70 Ru1 P40 175.683(11) . . ?
C31 Ru1 Cl20 92.89(4) . . ?
N1 Ru1 Cl20 170.41(3) . . ?
O16 Ru1 Cl20 84.96(3) . . ?
P70 Ru1 Cl20 92.029(11) . . ?
P40 Ru1 Cl20 91.576(11) . . ?
C2 N1 Ru1 129.07(8) . . ?
N1 C2 C3 118.11(10) . . ?
N1 C2 C15 124.60(10) . . ?
C3 C2 C15 117.28(10) . . ?
C4 C3 C2 122.05(12) . . ?
C3 C4 C5 120.65(12) . . ?
C6 C5 C4 119.80(11) . . ?
C5 C6 C15 121.59(11) . . ?
C5 C6 C7 117.52(11) . . ?
C15 C6 C7 120.87(11) . . ?
O17 C7 C8 121.10(12) . . ?
O17 C7 C6 121.53(12) . . ?
C8 C7 C6 117.37(10) . . ?
C9 C8 C13 119.96(12) . . ?
C9 C8 C7 119.76(11) . . ?
C13 C8 C7 120.26(11) . . ?
C10 C9 C8 120.27(12) . . ?
C9 C10 C11 119.94(12) . . ?
C12 C11 C10 120.31(13) . . ?
C11 C12 C13 120.19(12) . . ?
C8 C13 C12 119.31(11) . . ?
C8 C13 C14 120.81(11) . . ?
C12 C13 C14 119.83(10) . . ?
O16 C14 C15 125.33(10) . . ?
O16 C14 C13 114.79(10) . . ?
C15 C14 C13 119.87(10) . . ?
C14 C15 C6 119.70(10) . . ?
C14 C15 C2 122.09(10) . . ?
C6 C15 C2 118.10(10) . . ?
C14 O16 Ru1 128.58(7) . . ?
O32 C31 Ru1 178.55(11) . . ?
C51 P40 C41 105.22(6) . . ?
C51 P40 C61 103.61(5) . . ?
C41 P40 C61 101.36(5) . . ?
C51 P40 Ru1 109.69(4) . . ?
C41 P40 Ru1 120.12(4) . . ?
C61 P40 Ru1 115.17(4) . . ?
C46 C41 C42 119.46(11) . . ?
C46 C41 P40 120.56(9) . . ?
C42 C41 P40 119.97(9) . . ?
C43 C42 C41 120.03(12) . . ?
C42 C43 C44 120.02(13) . . ?
C45 C44 C43 120.08(12) . . ?
C44 C45 C46 120.12(12) . . ?
C41 C46 C45 120.24(11) . . ?
C52 C51 C56 118.95(11) . . ?
C52 C51 P40 123.33(9) . . ?
C56 C51 P40 117.36(9) . . ?
C51 C52 C53 119.76(12) . . ?
C54 C53 C52 120.91(12) . . ?
C53 C54 C55 119.51(12) . . ?
C56 C55 C54 120.05(12) . . ?
C55 C56 C51 120.81(11) . . ?
C66 C61 C62 118.68(11) . . ?
C66 C61 P40 122.70(9) . . ?
C62 C61 P40 118.60(9) . . ?
C63 C62 C61 120.36(12) . . ?
C64 C63 C62 120.59(12) . . ?
C65 C64 C63 119.34(11) . . ?
C64 C65 C66 120.61(12) . . ?
C61 C66 C65 120.39(12) . . ?
C91 P70 C81 102.28(6) . . ?
C91 P70 C71 104.04(6) . . ?
C81 P70 C71 104.45(6) . . ?
C91 P70 Ru1 118.13(4) . . ?
C81 P70 Ru1 115.38(4) . . ?
C71 P70 Ru1 111.06(4) . . ?
C72 C71 C76 118.72(11) . . ?
C72 C71 P70 121.99(9) . . ?
C76 C71 P70 118.77(9) . . ?
C73 C72 C71 120.28(12) . . ?
C74 C73 C72 120.48(12) . . ?
C73 C74 C75 119.63(12) . . ?
C76 C75 C74 120.21(13) . . ?
C75 C76 C71 120.69(12) . . ?
C86 C81 C82 119.53(11) . . ?
C86 C81 P70 117.03(9) . . ?
C82 C81 P70 123.37(10) . . ?
C83 C82 C81 120.25(13) . . ?
C84 C83 C82 120.01(13) . . ?
C83 C84 C85 119.94(12) . . ?
C86 C85 C84 120.53(13) . . ?
C85 C86 C81 119.73(12) . . ?
C96 C91 C92 119.06(11) . . ?
C96 C91 P70 121.26(9) . . ?
C92 C91 P70 119.68(9) . . ?
C93 C92 C91 120.10(12) . . ?
C92 C93 C94 120.40(12) . . ?
C95 C94 C93 119.88(12) . . ?
C94 C95 C96 119.95(12) . . ?
C95 C96 C91 120.59(11) . . ?

_refine_diff_density_max         1.116
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.083

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_2_I5_295K
_database_code_depnum_ccdc_archive 'CCDC 1447878'
_audit_update_record             
;
2016-11-21 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C51 H38 Br I6 N O3 Os P2'
_chemical_formula_weight         1806.27

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   12.1385(8)
_cell_length_b                   15.2266(10)
_cell_length_c                   15.6850(10)
_cell_angle_alpha                73.594(3)
_cell_angle_beta                 80.258(3)
_cell_angle_gamma                77.265(3)
_cell_volume                     2694.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    9818
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      26.46

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.226
_exptl_crystal_F_000             1668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    6.644
_shelx_estimated_absorpt_T_min   0.336
_shelx_estimated_absorpt_T_max   0.556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.315
_exptl_absorpt_correction_T_max  0.520
_exptl_absorpt_process_details   'APEX2 (Bruker AXS Inc. 2007)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   Mo
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36736
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.430
_diffrn_reflns_theta_max         26.518
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             11115
_reflns_number_gt                8479
_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-97 (Sheldrick 2008)'
_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)+(0.1118P)²+37.0817P] 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     SHELXL
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11115
_refine_ls_number_parameters     587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0706
_refine_ls_wR_factor_ref         0.2166
_refine_ls_wR_factor_gt          0.1890
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.51479(3) 0.79531(3) 0.37976(3) 0.02901(16) Uani 1 1 d . . . . .
Br1 Br 0.50117(10) 0.85817(8) 0.51473(7) 0.0399(3) Uani 1 1 d . . . . .
I2 I 0.39005(12) 0.48487(8) 0.89905(9) 0.0809(4) Uani 1 1 d . . . . .
I4 I 0.10257(13) 0.38071(10) 1.07884(8) 0.0938(5) Uani 1 1 d . . . . .
I1 I 0.47433(14) 0.49691(11) 0.71939(10) 0.0963(5) Uani 1 1 d . . . . .
I3 I 0.29837(19) 0.46150(18) 1.09512(11) 0.1333(7) Uani 1 1 d . . . . .
I5 I -0.0822(2) 0.30048(16) 1.06738(15) 0.1362(7) Uani 1 1 d . . . . .
I6 I 0.9868(2) 0.08851(17) 0.01308(14) 0.1383(7) Uani 1 1 d . . . . .
P60 P 0.7204(2) 0.75428(18) 0.38448(18) 0.0294(6) Uani 1 1 d . . . . .
P30 P 0.3094(2) 0.83978(17) 0.38228(18) 0.0273(5) Uani 1 1 d . . . . .
O16 O 0.5321(6) 0.9288(5) 0.3028(5) 0.0320(16) Uani 1 1 d . . . . .
N1 N 0.5294(8) 0.7617(7) 0.2623(7) 0.041(2) Uani 1 1 d . . . . .
H1 H 0.5109 0.7097 0.2643 0.049 Uiso 1 1 calc R U . . .
O22 O 0.4806(9) 0.6019(6) 0.4756(7) 0.058(2) Uani 1 1 d . . . . .
C21 C 0.4953(8) 0.6710(8) 0.4402(7) 0.034(2) Uani 1 1 d . . . . .
C45 C 0.2669(12) 1.1207(9) 0.3421(11) 0.052(3) Uani 1 1 d . . . . .
H45 H 0.2815 1.1605 0.3725 0.062 Uiso 1 1 calc R U . . .
C15 C 0.5806(10) 0.9069(9) 0.1559(8) 0.041(3) Uani 1 1 d . . . . .
C3 C 0.5812(14) 0.7665(10) 0.1096(9) 0.053(3) Uani 1 1 d . . . . .
H3 H 0.5640 0.7073 0.1224 0.064 Uiso 1 1 calc R U . . .
C51 C 0.2238(10) 0.8222(8) 0.4920(7) 0.035(2) Uani 1 1 d . . . . .
C2 C 0.5656(12) 0.8132(8) 0.1799(8) 0.046(3) Uani 1 1 d . . . . .
C43 C 0.1975(12) 1.1002(10) 0.2203(10) 0.059(4) Uani 1 1 d . . . . .
H43 H 0.1664 1.1255 0.1665 0.071 Uiso 1 1 calc R U . . .
C12 C 0.5494(13) 1.1121(9) 0.2561(9) 0.051(3) Uani 1 1 d . . . . .
H12 H 0.5258 1.0848 0.3154 0.061 Uiso 1 1 calc R U . . .
C71 C 0.7953(9) 0.8518(8) 0.3415(8) 0.036(2) Uani 1 1 d . . . . .
C56 C 0.2634(10) 0.7599(9) 0.5677(8) 0.041(3) Uani 1 1 d . . . . .
H56 H 0.3380 0.7279 0.5652 0.049 Uiso 1 1 calc R U . . .
C76 C 0.7510(12) 0.9327(10) 0.3694(11) 0.057(4) Uani 1 1 d . . . . .
H76 H 0.6836 0.9370 0.4075 0.068 Uiso 1 1 calc R U . . .
C31 C 0.2506(9) 0.7741(8) 0.3262(8) 0.036(2) Uani 1 1 d . . . . .
C52 C 0.1121(11) 0.8694(9) 0.4963(9) 0.049(3) Uani 1 1 d . . . . .
H52 H 0.0837 0.9112 0.4457 0.058 Uiso 1 1 calc R U . . .
C6 C 0.6190(13) 0.9495(10) 0.0662(9) 0.051(3) Uani 1 1 d . . . . .
C13 C 0.5716(11) 1.0609(8) 0.1946(8) 0.043(3) Uani 1 1 d . . . . .
C81 C 0.7705(10) 0.7005(8) 0.4947(8) 0.040(3) Uani 1 1 d . . . . .
C62 C 0.8069(14) 0.6938(14) 0.2297(12) 0.074(5) Uani 1 1 d . . . . .
H62 H 0.7973 0.7561 0.1981 0.089 Uiso 1 1 calc R U . . .
C44 C 0.2188(12) 1.1569(9) 0.2630(10) 0.053(3) Uani 1 1 d . . . . .
H44 H 0.2015 1.2210 0.2398 0.063 Uiso 1 1 calc R U . . .
C4 C 0.6208(16) 0.8081(12) 0.0248(10) 0.071(5) Uani 1 1 d . . . . .
H4 H 0.6367 0.7749 -0.0187 0.085 Uiso 1 1 calc R U . . .
C41 C 0.2683(10) 0.9644(7) 0.3321(8) 0.037(3) Uani 1 1 d . . . . .
C14 C 0.5585(9) 0.9620(8) 0.2214(7) 0.034(2) Uani 1 1 d . . . . .
C33 C 0.2313(15) 0.7311(12) 0.1930(12) 0.068(4) Uani 1 1 d . . . . .
H33 H 0.2448 0.7401 0.1313 0.081 Uiso 1 1 calc R U . . .
C46 C 0.2939(10) 1.0236(9) 0.3773(10) 0.046(3) Uani 1 1 d . . . . .
H46 H 0.3283 0.9990 0.4297 0.055 Uiso 1 1 calc R U . . .
C11 C 0.5617(16) 1.2042(10) 0.2309(12) 0.069(4) Uani 1 1 d . . . . .
H11 H 0.5449 1.2397 0.2725 0.082 Uiso 1 1 calc R U . . .
C36 C 0.1923(12) 0.7041(9) 0.3770(9) 0.046(3) Uani 1 1 d . . . . .
H36 H 0.1783 0.6935 0.4389 0.055 Uiso 1 1 calc R U . . .
C42 C 0.2206(12) 1.0020(9) 0.2540(9) 0.049(3) Uani 1 1 d . . . . .
H42 H 0.2034 0.9637 0.2231 0.059 Uiso 1 1 calc R U . . .
C54 C 0.0846(14) 0.7914(11) 0.6526(10) 0.061(4) Uani 1 1 d . . . . .
H54 H 0.0382 0.7816 0.7068 0.073 Uiso 1 1 calc R U . . .
C75 C 0.8089(12) 1.0074(10) 0.3396(12) 0.064(4) Uani 1 1 d . . . . .
H75 H 0.7801 1.0611 0.3591 0.077 Uiso 1 1 calc R U . . .
C35 C 0.1548(16) 0.6495(13) 0.3323(14) 0.078(5) Uani 1 1 d . . . . .
H35 H 0.1172 0.6015 0.3655 0.093 Uiso 1 1 calc R U . . .
C53 C 0.0420(13) 0.8529(12) 0.5792(11) 0.065(4) Uani 1 1 d . . . . .
H53 H -0.0329 0.8842 0.5833 0.078 Uiso 1 1 calc R U . . .
C86 C 0.8837(13) 0.6988(12) 0.5034(11) 0.063(4) Uani 1 1 d . . . . .
H86 H 0.9301 0.7284 0.4553 0.076 Uiso 1 1 calc R U . . .
O17 O 0.6723(14) 1.0792(10) -0.0386(7) 0.097(5) Uani 1 1 d . . . . .
C32 C 0.2725(11) 0.7859(9) 0.2331(9) 0.047(3) Uani 1 1 d . . . . .
H32 H 0.3146 0.8303 0.1984 0.056 Uiso 1 1 calc R U . . .
C8 C 0.6107(13) 1.1003(9) 0.1054(9) 0.051(3) Uani 1 1 d . . . . .
C34 C 0.1722(15) 0.6655(12) 0.2421(13) 0.070(5) Uani 1 1 d . . . . .
H34 H 0.1432 0.6307 0.2140 0.085 Uiso 1 1 calc R U . . .
C83 C 0.7521(15) 0.6114(13) 0.6457(10) 0.069(4) Uani 1 1 d . . . . .
H83 H 0.7064 0.5815 0.6941 0.082 Uiso 1 1 calc R U . . .
C61 C 0.7817(12) 0.6669(11) 0.3231(10) 0.055(3) Uani 1 1 d . . . . .
C5 C 0.6378(15) 0.8990(12) 0.0021(9) 0.063(4) Uani 1 1 d . . . . .
H5 H 0.6621 0.9269 -0.0569 0.076 Uiso 1 1 calc R U . . .
C55 C 0.1918(13) 0.7445(10) 0.6488(10) 0.054(3) Uani 1 1 d . . . . .
H55 H 0.2187 0.7019 0.6996 0.065 Uiso 1 1 calc R U . . .
C64 C 0.862(2) 0.531(3) 0.230(3) 0.134(15) Uani 1 1 d . . . . .
H64 H 0.8924 0.4849 0.2008 0.160 Uiso 1 1 calc R U . . .
C84 C 0.8618(16) 0.6087(12) 0.6560(12) 0.071(5) Uani 1 1 d . . . . .
H84 H 0.8921 0.5784 0.7095 0.085 Uiso 1 1 calc R U . . .
C63 C 0.8482(18) 0.620(3) 0.1854(19) 0.128(12) Uani 1 1 d . . . . .
H63 H 0.8658 0.6353 0.1235 0.153 Uiso 1 1 calc R U . . .
C65 C 0.834(2) 0.5105(18) 0.313(3) 0.131(12) Uani 1 1 d . . . . .
H65 H 0.8374 0.4478 0.3418 0.158 Uiso 1 1 calc R U . . .
C66 C 0.7965(17) 0.5753(11) 0.3643(16) 0.086(6) Uani 1 1 d . . . . .
H66 H 0.7822 0.5553 0.4262 0.103 Uiso 1 1 calc R U . . .
C82 C 0.7057(13) 0.6559(10) 0.5678(9) 0.056(4) Uani 1 1 d . . . . .
H82 H 0.6299 0.6560 0.5642 0.067 Uiso 1 1 calc R U . . .
C72 C 0.8973(13) 0.8462(11) 0.2842(11) 0.060(4) Uani 1 1 d . . . . .
H72 H 0.9277 0.7923 0.2654 0.072 Uiso 1 1 calc R U . . .
C73 C 0.9519(15) 0.9211(14) 0.2563(12) 0.079(5) Uani 1 1 d . . . . .
H73 H 1.0202 0.9173 0.2191 0.095 Uiso 1 1 calc R U . . .
C85 C 0.9253(16) 0.6539(14) 0.5817(12) 0.080(5) Uani 1 1 d . . . . .
H85 H 1.0010 0.6534 0.5859 0.096 Uiso 1 1 calc R U . . .
C9 C 0.621(2) 1.1958(13) 0.0817(14) 0.095(7) Uani 1 1 d . . . . .
H9 H 0.6422 1.2245 0.0223 0.114 Uiso 1 1 calc R U . . .
C74 C 0.9061(16) 1.0033(14) 0.2830(13) 0.077(5) Uani 1 1 d . . . . .
H74 H 0.9422 1.0545 0.2620 0.093 Uiso 1 1 calc R U . . .
C7 C 0.6382(16) 1.0468(11) 0.0374(10) 0.067(4) Uani 1 1 d . . . . .
C10 C 0.600(2) 1.2437(12) 0.1407(14) 0.095(7) Uani 1 1 d . . . . .
H10 H 0.6109 1.3051 0.1235 0.114 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 C21 1.910(12) . ?
Os1 N1 2.017(11) . ?
Os1 O16 2.085(7) . ?
Os1 P30 2.432(3) . ?
Os1 P60 2.444(3) . ?
Os1 Br1 2.5262(12) . ?
I2 I1 2.799(2) . ?
I2 I3 3.037(2) . ?
I4 I5 2.832(3) . ?
I4 I3 2.983(3) . ?
I6 I6 2.781(5) 2_755 ?
P60 C61 1.816(14) . ?
P60 C71 1.820(11) . ?
P60 C81 1.835(12) . ?
P30 C31 1.819(12) . ?
P30 C41 1.828(11) . ?
P30 C51 1.836(11) . ?
O16 C14 1.248(13) . ?
N1 C2 1.366(15) . ?
N1 H1 0.8600 . ?
O22 C21 1.079(14) . ?
C45 C44 1.38(2) . ?
C45 C46 1.409(18) . ?
C45 H45 0.9300 . ?
C15 C2 1.413(17) . ?
C15 C6 1.418(18) . ?
C15 C14 1.457(16) . ?
C3 C4 1.36(2) . ?
C3 C2 1.439(17) . ?
C3 H3 0.9300 . ?
C51 C56 1.378(17) . ?
C51 C52 1.387(17) . ?
C43 C44 1.32(2) . ?
C43 C42 1.419(19) . ?
C43 H43 0.9300 . ?
C12 C13 1.363(19) . ?
C12 C11 1.380(19) . ?
C12 H12 0.9300 . ?
C71 C76 1.389(19) . ?
C71 C72 1.403(19) . ?
C56 C55 1.406(17) . ?
C56 H56 0.9300 . ?
C76 C75 1.395(19) . ?
C76 H76 0.9300 . ?
C31 C36 1.391(17) . ?
C31 C32 1.405(18) . ?
C52 C53 1.418(19) . ?
C52 H52 0.9300 . ?
C6 C5 1.391(19) . ?
C6 C7 1.48(2) . ?
C13 C8 1.402(17) . ?
C13 C14 1.481(16) . ?
C81 C82 1.373(18) . ?
C81 C86 1.398(19) . ?
C62 C61 1.40(2) . ?
C62 C63 1.44(3) . ?
C62 H62 0.9300 . ?
C44 H44 0.9300 . ?
C4 C5 1.38(2) . ?
C4 H4 0.9300 . ?
C41 C42 1.365(18) . ?
C41 C46 1.403(18) . ?
C33 C34 1.34(2) . ?
C33 C32 1.39(2) . ?
C33 H33 0.9300 . ?
C46 H46 0.9300 . ?
C11 C10 1.42(3) . ?
C11 H11 0.9300 . ?
C36 C35 1.41(2) . ?
C36 H36 0.9300 . ?
C42 H42 0.9300 . ?
C54 C55 1.34(2) . ?
C54 C53 1.36(2) . ?
C54 H54 0.9300 . ?
C75 C74 1.35(2) . ?
C75 H75 0.9300 . ?
C35 C34 1.35(3) . ?
C35 H35 0.9300 . ?
C53 H53 0.9300 . ?
C86 C85 1.35(2) . ?
C86 H86 0.9300 . ?
O17 C7 1.195(17) . ?
C32 H32 0.9300 . ?
C8 C9 1.42(2) . ?
C8 C7 1.47(2) . ?
C34 H34 0.9300 . ?
C83 C84 1.36(2) . ?
C83 C82 1.37(2) . ?
C83 H83 0.9300 . ?
C61 C66 1.35(2) . ?
C5 H5 0.9300 . ?
C55 H55 0.9300 . ?
C64 C65 1.24(5) . ?
C64 C63 1.33(5) . ?
C64 H64 0.9300 . ?
C84 C85 1.38(3) . ?
C84 H84 0.9300 . ?
C63 H63 0.9300 . ?
C65 C66 1.40(3) . ?
C65 H65 0.9300 . ?
C66 H66 0.9300 . ?
C82 H82 0.9300 . ?
C72 C73 1.37(2) . ?
C72 H72 0.9300 . ?
C73 C74 1.40(3) . ?
C73 H73 0.9300 . ?
C85 H85 0.9300 . ?
C9 C10 1.29(3) . ?
C9 H9 0.9300 . ?
C74 H74 0.9300 . ?
C10 H10 0.9300 . ?

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
C21 Os1 N1 88.8(4) . . ?
C21 Os1 O16 174.5(4) . . ?
N1 Os1 O16 86.0(3) . . ?
C21 Os1 P30 88.7(3) . . ?
N1 Os1 P30 91.5(3) . . ?
O16 Os1 P30 89.8(2) . . ?
C21 Os1 P60 91.9(3) . . ?
N1 Os1 P60 91.7(3) . . ?
O16 Os1 P60 90.0(2) . . ?
P30 Os1 P60 176.76(9) . . ?
C21 Os1 Br1 98.7(4) . . ?
N1 Os1 Br1 172.5(3) . . ?
O16 Os1 Br1 86.5(2) . . ?
P30 Os1 Br1 88.93(7) . . ?
P60 Os1 Br1 87.83(7) . . ?
I1 I2 I3 177.10(7) . . ?
I5 I4 I3 178.56(8) . . ?
I4 I3 I2 93.51(6) . . ?
C61 P60 C71 108.6(6) . . ?
C61 P60 C81 102.9(6) . . ?
C71 P60 C81 102.4(6) . . ?
C61 P60 Os1 110.2(5) . . ?
C71 P60 Os1 114.7(4) . . ?
C81 P60 Os1 117.1(4) . . ?
C31 P30 C41 109.7(6) . . ?
C31 P30 C51 102.2(5) . . ?
C41 P30 C51 103.3(5) . . ?
C31 P30 Os1 112.6(4) . . ?
C41 P30 Os1 110.8(4) . . ?
C51 P30 Os1 117.5(4) . . ?
C14 O16 Os1 133.4(7) . . ?
C2 N1 Os1 126.6(9) . . ?
C2 N1 H1 116.7 . . ?
Os1 N1 H1 116.7 . . ?
O22 C21 Os1 177.4(10) . . ?
C44 C45 C46 120.3(13) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C2 C15 C6 120.0(11) . . ?
C2 C15 C14 121.8(11) . . ?
C6 C15 C14 118.2(11) . . ?
C4 C3 C2 120.7(13) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C56 C51 C52 119.4(11) . . ?
C56 C51 P30 122.7(9) . . ?
C52 C51 P30 117.7(9) . . ?
N1 C2 C15 127.8(11) . . ?
N1 C2 C3 114.2(11) . . ?
C15 C2 C3 117.8(11) . . ?
C44 C43 C42 122.1(14) . . ?
C44 C43 H43 118.9 . . ?
C42 C43 H43 118.9 . . ?
C13 C12 C11 120.4(13) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C76 C71 C72 119.7(11) . . ?
C76 C71 P60 118.2(9) . . ?
C72 C71 P60 122.1(10) . . ?
C51 C56 C55 120.5(12) . . ?
C51 C56 H56 119.8 . . ?
C55 C56 H56 119.8 . . ?
C71 C76 C75 119.2(13) . . ?
C71 C76 H76 120.4 . . ?
C75 C76 H76 120.4 . . ?
C36 C31 C32 118.9(11) . . ?
C36 C31 P30 119.4(9) . . ?
C32 C31 P30 121.4(9) . . ?
C51 C52 C53 119.0(13) . . ?
C51 C52 H52 120.5 . . ?
C53 C52 H52 120.5 . . ?
C5 C6 C15 119.2(13) . . ?
C5 C6 C7 118.3(13) . . ?
C15 C6 C7 122.5(12) . . ?
C12 C13 C8 120.4(11) . . ?
C12 C13 C14 120.5(11) . . ?
C8 C13 C14 119.0(11) . . ?
C82 C81 C86 117.8(13) . . ?
C82 C81 P60 123.8(10) . . ?
C86 C81 P60 118.2(10) . . ?
C61 C62 C63 117(2) . . ?
C61 C62 H62 121.6 . . ?
C63 C62 H62 121.6 . . ?
C43 C44 C45 119.8(12) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C3 C4 C5 121.0(13) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C42 C41 C46 119.4(11) . . ?
C42 C41 P30 125.0(10) . . ?
C46 C41 P30 115.6(9) . . ?
O16 C14 C15 122.8(10) . . ?
O16 C14 C13 116.1(10) . . ?
C15 C14 C13 121.0(10) . . ?
C34 C33 C32 120.9(16) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C41 C46 C45 119.2(12) . . ?
C41 C46 H46 120.4 . . ?
C45 C46 H46 120.4 . . ?
C12 C11 C10 118.8(15) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
C31 C36 C35 118.3(13) . . ?
C31 C36 H36 120.9 . . ?
C35 C36 H36 120.9 . . ?
C41 C42 C43 119.2(13) . . ?
C41 C42 H42 120.4 . . ?
C43 C42 H42 120.4 . . ?
C55 C54 C53 121.6(13) . . ?
C55 C54 H54 119.2 . . ?
C53 C54 H54 119.2 . . ?
C74 C75 C76 121.4(15) . . ?
C74 C75 H75 119.3 . . ?
C76 C75 H75 119.3 . . ?
C34 C35 C36 121.5(16) . . ?
C34 C35 H35 119.2 . . ?
C36 C35 H35 119.2 . . ?
C54 C53 C52 119.9(14) . . ?
C54 C53 H53 120.1 . . ?
C52 C53 H53 120.1 . . ?
C85 C86 C81 119.6(15) . . ?
C85 C86 H86 120.2 . . ?
C81 C86 H86 120.2 . . ?
C33 C32 C31 120.0(13) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C13 C8 C9 117.5(14) . . ?
C13 C8 C7 122.1(12) . . ?
C9 C8 C7 120.3(14) . . ?
C33 C34 C35 120.3(14) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C84 C83 C82 123.2(15) . . ?
C84 C83 H83 118.4 . . ?
C82 C83 H83 118.4 . . ?
C66 C61 C62 118.4(15) . . ?
C66 C61 P60 121.4(14) . . ?
C62 C61 P60 120.0(13) . . ?
C4 C5 C6 121.0(13) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C54 C55 C56 119.7(14) . . ?
C54 C55 H55 120.1 . . ?
C56 C55 H55 120.1 . . ?
C65 C64 C63 120(2) . . ?
C65 C64 H64 120.2 . . ?
C63 C64 H64 120.2 . . ?
C83 C84 C85 115.6(15) . . ?
C83 C84 H84 122.2 . . ?
C85 C84 H84 122.2 . . ?
C64 C63 C62 122(3) . . ?
C64 C63 H63 119.2 . . ?
C62 C63 H63 119.2 . . ?
C64 C65 C66 124(3) . . ?
C64 C65 H65 117.8 . . ?
C66 C65 H65 117.8 . . ?
C61 C66 C65 119(2) . . ?
C61 C66 H66 120.4 . . ?
C65 C66 H66 120.4 . . ?
C83 C82 C81 120.2(14) . . ?
C83 C82 H82 119.9 . . ?
C81 C82 H82 119.9 . . ?
C73 C72 C71 119.4(15) . . ?
C73 C72 H72 120.3 . . ?
C71 C72 H72 120.3 . . ?
C72 C73 C74 120.9(15) . . ?
C72 C73 H73 119.5 . . ?
C74 C73 H73 119.5 . . ?
C86 C85 C84 123.6(17) . . ?
C86 C85 H85 118.2 . . ?
C84 C85 H85 118.2 . . ?
C10 C9 C8 121.6(17) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C75 C74 C73 119.3(15) . . ?
C75 C74 H74 120.4 . . ?
C73 C74 H74 120.4 . . ?
O17 C7 C8 123.0(15) . . ?
O17 C7 C6 120.0(15) . . ?
C8 C7 C6 117.0(12) . . ?
C9 C10 C11 121.2(15) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?

_refine_diff_density_max         3.306
_refine_diff_density_min         -2.250
_refine_diff_density_rms         0.355

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_ANQRuP
_database_code_depnum_ccdc_archive 'CCDC 1490059'
_audit_update_record             
;
2016-07-02 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H38 Cl2 N O2 P2 Ru'
_chemical_formula_weight         918.72

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'
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'
Ru Ru -1.2594 0.8363 '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                   9.6319(5)
_cell_length_b                   17.1986(9)
_cell_length_c                   25.4291(13)
_cell_angle_alpha                90
_cell_angle_beta                 98.221(2)
_cell_angle_gamma                90
_cell_volume                     4169.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9661
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.66

_exptl_crystal_description       Prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_F_000             1876
_exptl_transmission_factor_min   0.820
_exptl_transmission_factor_max   0.942
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.624
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51063
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.005
_diffrn_reflns_theta_max         27.865
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9777
_reflns_number_gt                7824
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.0356P)²+2.2375P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9777
_refine_ls_number_parameters     526
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0832
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
C2 C 0.6543(2) 0.80037(12) 0.65281(9) 0.0333(5) Uani 1 1 d . . . . .
C3 C 0.8020(2) 0.80316(15) 0.65128(11) 0.0461(6) Uani 1 1 d . . . . .
H3 H 0.8343 0.8067 0.6186 0.055 Uiso 1 1 calc R U . . .
C4 C 0.8965(3) 0.80070(17) 0.69651(12) 0.0568(7) Uani 1 1 d . . . . .
H4 H 0.9921 0.8032 0.6945 0.068 Uiso 1 1 calc R U . . .
C5 C 0.8507(3) 0.79452(16) 0.74575(11) 0.0528(7) Uani 1 1 d . . . . .
H5 H 0.9161 0.7952 0.7764 0.063 Uiso 1 1 calc R U . . .
C6 C 0.7113(2) 0.78749(14) 0.74993(9) 0.0398(5) Uani 1 1 d . . . . .
C7 C 0.6688(3) 0.77660(15) 0.80338(10) 0.0472(6) Uani 1 1 d . . . . .
C8 C 0.5231(3) 0.75469(14) 0.80654(9) 0.0418(5) Uani 1 1 d . . . . .
C9 C 0.4814(3) 0.73790(17) 0.85527(10) 0.0569(7) Uani 1 1 d . . . . .
H9 H 0.5458 0.7417 0.8861 0.068 Uiso 1 1 calc R U . . .
C10 C 0.3466(3) 0.71581(19) 0.85843(11) 0.0658(8) Uani 1 1 d . . . . .
H10 H 0.3203 0.7043 0.8914 0.079 Uiso 1 1 calc R U . . .
C11 C 0.2484(3) 0.71032(18) 0.81287(11) 0.0593(7) Uani 1 1 d . . . . .
H11 H 0.1567 0.6954 0.8153 0.071 Uiso 1 1 calc R U . . .
C12 C 0.2878(3) 0.72708(15) 0.76415(10) 0.0464(6) Uani 1 1 d . . . . .
H12 H 0.2223 0.7233 0.7336 0.056 Uiso 1 1 calc R U . . .
C13 C 0.4252(2) 0.74968(13) 0.76006(8) 0.0363(5) Uani 1 1 d . . . . .
C14 C 0.4658(2) 0.77077(12) 0.70814(8) 0.0314(4) Uani 1 1 d . . . . .
C15 C 0.6075(2) 0.78848(12) 0.70341(8) 0.0317(4) Uani 1 1 d . . . . .
C31 C 0.2941(2) 1.02313(13) 0.58194(9) 0.0359(5) Uani 1 1 d . . . . .
C32 C 0.1501(3) 1.01965(17) 0.56754(13) 0.0617(8) Uani 1 1 d . . . . .
H32 H 0.1001 0.9779 0.5786 0.074 Uiso 1 1 calc R U . . .
C33 C 0.0798(3) 1.07794(18) 0.53674(14) 0.0693(9) Uani 1 1 d . . . . .
H33 H -0.0172 1.0754 0.5277 0.083 Uiso 1 1 calc R U . . .
C34 C 0.1518(3) 1.13877(15) 0.51972(10) 0.0493(6) Uani 1 1 d . . . . .
H34 H 0.1043 1.1780 0.4994 0.059 Uiso 1 1 calc R U . . .
C35 C 0.2933(3) 1.14193(15) 0.53256(10) 0.0502(6) Uani 1 1 d . . . . .
H35 H 0.3425 1.1832 0.5204 0.060 Uiso 1 1 calc R U . . .
C36 C 0.3654(2) 1.08484(14) 0.56345(10) 0.0450(6) Uani 1 1 d . . . . .
H36 H 0.4624 1.0879 0.5719 0.054 Uiso 1 1 calc R U . . .
C41 C 0.3179(2) 0.97518(14) 0.68898(9) 0.0397(5) Uani 1 1 d . . . . .
C42 C 0.2475(3) 0.92188(15) 0.71570(10) 0.0463(6) Uani 1 1 d . . . . .
H42 H 0.2299 0.8723 0.7017 0.056 Uiso 1 1 calc R U . . .
C43 C 0.2023(3) 0.94196(18) 0.76357(11) 0.0646(8) Uani 1 1 d . . . . .
H43 H 0.1561 0.9054 0.7817 0.078 Uiso 1 1 calc R U . . .
C44 C 0.2256(4) 1.0148(2) 0.78390(13) 0.0749(10) Uani 1 1 d . . . . .
H44 H 0.1955 1.0279 0.8159 0.090 Uiso 1 1 calc R U . . .
C45 C 0.2933(4) 1.06866(19) 0.75728(13) 0.0840(11) Uani 1 1 d . . . . .
H45 H 0.3088 1.1185 0.7711 0.101 Uiso 1 1 calc R U . . .
C46 C 0.3387(4) 1.04906(17) 0.70966(12) 0.0715(9) Uani 1 1 d . . . . .
H46 H 0.3837 1.0861 0.6915 0.086 Uiso 1 1 calc R U . . .
C51 C 0.5656(2) 0.97772(13) 0.63586(9) 0.0349(5) Uani 1 1 d . . . . .
C52 C 0.6343(2) 0.97819(14) 0.59129(9) 0.0420(5) Uani 1 1 d . . . . .
H52 H 0.5843 0.9673 0.5581 0.050 Uiso 1 1 calc R U . . .
C53 C 0.7754(3) 0.99462(17) 0.59577(11) 0.0555(7) Uani 1 1 d . . . . .
H53 H 0.8197 0.9955 0.5656 0.067 Uiso 1 1 calc R U . . .
C54 C 0.8511(3) 1.00973(18) 0.64495(13) 0.0637(8) Uani 1 1 d . . . . .
H54 H 0.9462 1.0213 0.6480 0.076 Uiso 1 1 calc R U . . .
C55 C 0.7858(3) 1.00765(19) 0.68883(12) 0.0640(8) Uani 1 1 d . . . . .
H55 H 0.8373 1.0172 0.7220 0.077 Uiso 1 1 calc R U . . .
C56 C 0.6433(3) 0.99149(15) 0.68503(10) 0.0478(6) Uani 1 1 d . . . . .
H56 H 0.6003 0.9899 0.7155 0.057 Uiso 1 1 calc R U . . .
C61 C 0.3090(3) 0.60799(14) 0.60423(9) 0.0425(5) Uani 1 1 d . . . . .
C62 C 0.3839(3) 0.53966(16) 0.61195(12) 0.0618(7) Uani 1 1 d . . . . .
H62 H 0.4606 0.5313 0.5942 0.074 Uiso 1 1 calc R U . . .
C63 C 0.3451(4) 0.48332(19) 0.64621(13) 0.0768(10) Uani 1 1 d . . . . .
H63 H 0.3970 0.4377 0.6518 0.092 Uiso 1 1 calc R U . . .
C64 C 0.2325(4) 0.4944(2) 0.67135(12) 0.0752(10) Uani 1 1 d . . . . .
H64 H 0.2068 0.4563 0.6940 0.090 Uiso 1 1 calc R U . . .
C65 C 0.1554(4) 0.5621(2) 0.66358(12) 0.0721(9) Uani 1 1 d . . . . .
H65 H 0.0771 0.5694 0.6806 0.087 Uiso 1 1 calc R U . . .
C66 C 0.1954(3) 0.61923(17) 0.63021(11) 0.0559(7) Uani 1 1 d . . . . .
H66 H 0.1448 0.6654 0.6255 0.067 Uiso 1 1 calc R U . . .
C71 C 0.2223(2) 0.66331(14) 0.49934(9) 0.0390(5) Uani 1 1 d . . . . .
C72 C 0.1406(2) 0.72062(15) 0.47283(9) 0.0404(5) Uani 1 1 d . . . . .
H72 H 0.1485 0.7715 0.4852 0.048 Uiso 1 1 calc R U . . .
C73 C 0.0468(3) 0.70325(16) 0.42791(10) 0.0489(6) Uani 1 1 d . . . . .
H73 H -0.0075 0.7425 0.4102 0.059 Uiso 1 1 calc R U . . .
C74 C 0.0338(3) 0.62908(18) 0.40968(11) 0.0642(8) Uani 1 1 d . . . . .
H74 H -0.0286 0.6177 0.3793 0.077 Uiso 1 1 calc R U . . .
C75 C 0.1119(4) 0.57152(19) 0.43579(14) 0.0827(11) Uani 1 1 d . . . . .
H75 H 0.1013 0.5206 0.4236 0.099 Uiso 1 1 calc R U . . .
C76 C 0.2074(3) 0.58838(17) 0.48063(12) 0.0686(9) Uani 1 1 d . . . . .
H76 H 0.2614 0.5488 0.4980 0.082 Uiso 1 1 calc R U . . .
C81 C 0.5184(2) 0.65664(13) 0.53986(9) 0.0376(5) Uani 1 1 d . . . . .
C82 C 0.6322(3) 0.64498(15) 0.57977(10) 0.0475(6) Uani 1 1 d . . . . .
H82 H 0.6178 0.6448 0.6152 0.057 Uiso 1 1 calc R U . . .
C83 C 0.7657(3) 0.63375(17) 0.56735(13) 0.0630(8) Uani 1 1 d . . . . .
H83 H 0.8403 0.6261 0.5944 0.076 Uiso 1 1 calc R U . . .
C84 C 0.7891(3) 0.63379(18) 0.51562(15) 0.0695(9) Uani 1 1 d . . . . .
H84 H 0.8792 0.6263 0.5074 0.083 Uiso 1 1 calc R U . . .
C85 C 0.6789(3) 0.64498(18) 0.47582(13) 0.0660(8) Uani 1 1 d . . . . .
H85 H 0.6946 0.6449 0.4406 0.079 Uiso 1 1 calc R U . . .
C86 C 0.5436(3) 0.65650(16) 0.48768(10) 0.0509(6) Uani 1 1 d . . . . .
H86 H 0.4698 0.6641 0.4603 0.061 Uiso 1 1 calc R U . . .
Cl1 Cl 0.36838(6) 0.86268(4) 0.51039(2) 0.04133(13) Uani 1 1 d . . . . .
Cl2 Cl 0.11095(5) 0.81799(4) 0.59102(2) 0.04221(13) Uani 1 1 d . . . . .
H1 H 0.608(3) 0.8100(14) 0.5789(11) 0.051 Uiso 1 1 d . U . . .
N1 N 0.56678(18) 0.80671(10) 0.60764(7) 0.0321(4) Uani 1 1 d . . . . .
O16 O 0.36562(14) 0.77001(9) 0.66963(5) 0.0323(3) Uani 1 1 d . . . . .
O17 O 0.7541(2) 0.78563(15) 0.84348(8) 0.0766(6) Uani 1 1 d . . . . .
P30 P 0.38118(6) 0.94883(3) 0.62675(2) 0.03167(12) Uani 1 1 d . . . . .
P60 P 0.34873(6) 0.68441(3) 0.55835(2) 0.03150(12) Uani 1 1 d . . . . .
Ru1 Ru 0.36038(2) 0.81415(2) 0.59598(2) 0.02751(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 N1 1.329(3) . ?
C2 C3 1.429(3) . ?
C2 C15 1.438(3) . ?
C3 C4 1.362(4) . ?
C4 C5 1.390(4) . ?
C5 C6 1.368(3) . ?
C6 C15 1.436(3) . ?
C6 C7 1.486(3) . ?
C7 O17 1.224(3) . ?
C7 C8 1.467(4) . ?
C8 C9 1.386(3) . ?
C8 C13 1.405(3) . ?
C9 C10 1.366(4) . ?
C10 C11 1.390(4) . ?
C11 C12 1.377(3) . ?
C12 C13 1.397(3) . ?
C13 C14 1.475(3) . ?
C14 O16 1.272(2) . ?
C14 C15 1.420(3) . ?
C31 C36 1.383(3) . ?
C31 C32 1.384(3) . ?
C31 P30 1.833(2) . ?
C32 C33 1.388(4) . ?
C33 C34 1.360(4) . ?
C34 C35 1.356(4) . ?
C35 C36 1.381(3) . ?
C41 C42 1.376(3) . ?
C41 C46 1.379(4) . ?
C41 P30 1.832(2) . ?
C42 C43 1.393(3) . ?
C43 C44 1.361(4) . ?
C44 C45 1.366(4) . ?
C45 C46 1.387(4) . ?
C51 C56 1.383(3) . ?
C51 C52 1.392(3) . ?
C51 P30 1.827(2) . ?
C52 C53 1.376(3) . ?
C53 C54 1.379(4) . ?
C54 C55 1.357(4) . ?
C55 C56 1.390(4) . ?
C61 C66 1.370(4) . ?
C61 C62 1.378(4) . ?
C61 P60 1.834(2) . ?
C62 C63 1.390(4) . ?
C63 C64 1.349(5) . ?
C64 C65 1.379(5) . ?
C65 C66 1.389(4) . ?
C71 C76 1.374(4) . ?
C71 C72 1.376(3) . ?
C71 P60 1.828(2) . ?
C72 C73 1.384(3) . ?
C73 C74 1.357(4) . ?
C74 C75 1.358(4) . ?
C75 C76 1.389(4) . ?
C81 C86 1.383(3) . ?
C81 C82 1.398(3) . ?
C81 P60 1.827(2) . ?
C82 C83 1.381(4) . ?
C83 C84 1.366(4) . ?
C84 C85 1.371(4) . ?
C85 C86 1.393(4) . ?
Cl1 Ru1 2.3427(5) . ?
Cl2 Ru1 2.3886(5) . ?
N1 Ru1 1.9717(17) . ?
O16 Ru1 2.0148(13) . ?
P30 Ru1 2.4439(6) . ?
P60 Ru1 2.4242(6) . ?

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
N1 C2 C3 119.0(2) . . ?
N1 C2 C15 122.92(18) . . ?
C3 C2 C15 118.0(2) . . ?
C4 C3 C2 121.6(2) . . ?
C3 C4 C5 120.2(2) . . ?
C6 C5 C4 121.2(2) . . ?
C5 C6 C15 120.7(2) . . ?
C5 C6 C7 119.0(2) . . ?
C15 C6 C7 120.3(2) . . ?
O17 C7 C8 121.3(2) . . ?
O17 C7 C6 120.4(2) . . ?
C8 C7 C6 118.26(19) . . ?
C9 C8 C13 119.6(2) . . ?
C9 C8 C7 120.3(2) . . ?
C13 C8 C7 120.1(2) . . ?
C10 C9 C8 120.6(2) . . ?
C9 C10 C11 120.6(2) . . ?
C12 C11 C10 119.5(3) . . ?
C11 C12 C13 120.7(2) . . ?
C12 C13 C8 118.9(2) . . ?
C12 C13 C14 120.64(19) . . ?
C8 C13 C14 120.5(2) . . ?
O16 C14 C15 124.68(19) . . ?
O16 C14 C13 114.71(18) . . ?
C15 C14 C13 120.60(18) . . ?
C14 C15 C6 119.5(2) . . ?
C14 C15 C2 122.33(18) . . ?
C6 C15 C2 117.92(19) . . ?
C36 C31 C32 118.1(2) . . ?
C36 C31 P30 122.74(17) . . ?
C32 C31 P30 119.10(18) . . ?
C31 C32 C33 120.5(2) . . ?
C34 C33 C32 120.3(3) . . ?
C35 C34 C33 119.7(2) . . ?
C34 C35 C36 121.0(2) . . ?
C35 C36 C31 120.4(2) . . ?
C42 C41 C46 118.7(2) . . ?
C42 C41 P30 120.67(18) . . ?
C46 C41 P30 120.61(19) . . ?
C41 C42 C43 120.2(2) . . ?
C44 C43 C42 120.3(3) . . ?
C43 C44 C45 120.0(3) . . ?
C44 C45 C46 120.0(3) . . ?
C41 C46 C45 120.7(3) . . ?
C56 C51 C52 118.4(2) . . ?
C56 C51 P30 123.50(17) . . ?
C52 C51 P30 117.74(17) . . ?
C53 C52 C51 120.8(2) . . ?
C52 C53 C54 120.1(2) . . ?
C55 C54 C53 119.6(3) . . ?
C54 C55 C56 121.1(3) . . ?
C51 C56 C55 119.9(2) . . ?
C66 C61 C62 119.3(2) . . ?
C66 C61 P60 117.3(2) . . ?
C62 C61 P60 123.3(2) . . ?
C61 C62 C63 120.1(3) . . ?
C64 C63 C62 120.4(3) . . ?
C63 C64 C65 120.3(3) . . ?
C64 C65 C66 119.6(3) . . ?
C61 C66 C65 120.3(3) . . ?
C76 C71 C72 118.5(2) . . ?
C76 C71 P60 119.66(19) . . ?
C72 C71 P60 121.81(18) . . ?
C71 C72 C73 120.7(2) . . ?
C74 C73 C72 120.1(2) . . ?
C73 C74 C75 120.1(3) . . ?
C74 C75 C76 120.3(3) . . ?
C71 C76 C75 120.3(3) . . ?
C86 C81 C82 118.0(2) . . ?
C86 C81 P60 122.24(19) . . ?
C82 C81 P60 119.23(18) . . ?
C83 C82 C81 120.9(3) . . ?
C84 C83 C82 120.5(3) . . ?
C83 C84 C85 119.6(3) . . ?
C84 C85 C86 120.6(3) . . ?
C81 C86 C85 120.4(3) . . ?
C2 N1 Ru1 129.57(15) . . ?
C14 O16 Ru1 128.82(13) . . ?
C51 P30 C41 105.10(10) . . ?
C51 P30 C31 103.85(10) . . ?
C41 P30 C31 100.69(10) . . ?
C51 P30 Ru1 109.39(7) . . ?
C41 P30 Ru1 119.26(8) . . ?
C31 P30 Ru1 116.89(8) . . ?
C81 P60 C71 104.61(11) . . ?
C81 P60 C61 104.59(11) . . ?
C71 P60 C61 101.82(11) . . ?
C81 P60 Ru1 110.46(8) . . ?
C71 P60 Ru1 119.63(8) . . ?
C61 P60 Ru1 114.24(8) . . ?
N1 Ru1 O16 86.86(7) . . ?
N1 Ru1 Cl1 89.79(6) . . ?
O16 Ru1 Cl1 176.48(4) . . ?
N1 Ru1 Cl2 174.03(5) . . ?
O16 Ru1 Cl2 87.18(4) . . ?
Cl1 Ru1 Cl2 96.17(2) . . ?
N1 Ru1 P60 89.33(5) . . ?
O16 Ru1 P60 90.79(4) . . ?
Cl1 Ru1 P60 88.10(2) . . ?
Cl2 Ru1 P60 90.87(2) . . ?
N1 Ru1 P30 88.78(5) . . ?
O16 Ru1 P30 93.99(4) . . ?
Cl1 Ru1 P30 87.01(2) . . ?
Cl2 Ru1 P30 91.52(2) . . ?
P60 Ru1 P30 174.761(19) . . ?

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
N1 C2 C3 C4 176.8(2) . . . . ?
C15 C2 C3 C4 -5.0(4) . . . . ?
C2 C3 C4 C5 0.7(4) . . . . ?
C3 C4 C5 C6 2.8(4) . . . . ?
C4 C5 C6 C15 -1.8(4) . . . . ?
C4 C5 C6 C7 176.6(3) . . . . ?
C5 C6 C7 O17 11.1(4) . . . . ?
C15 C6 C7 O17 -170.6(2) . . . . ?
C5 C6 C7 C8 -168.8(2) . . . . ?
C15 C6 C7 C8 9.6(3) . . . . ?
O17 C7 C8 C9 -4.9(4) . . . . ?
C6 C7 C8 C9 174.9(2) . . . . ?
O17 C7 C8 C13 175.8(3) . . . . ?
C6 C7 C8 C13 -4.3(3) . . . . ?
C13 C8 C9 C10 0.7(4) . . . . ?
C7 C8 C9 C10 -178.6(3) . . . . ?
C8 C9 C10 C11 -0.5(5) . . . . ?
C9 C10 C11 C12 0.2(5) . . . . ?
C10 C11 C12 C13 -0.1(4) . . . . ?
C11 C12 C13 C8 0.3(4) . . . . ?
C11 C12 C13 C14 -177.4(2) . . . . ?
C9 C8 C13 C12 -0.6(4) . . . . ?
C7 C8 C13 C12 178.7(2) . . . . ?
C9 C8 C13 C14 177.2(2) . . . . ?
C7 C8 C13 C14 -3.6(3) . . . . ?
C12 C13 C14 O16 3.2(3) . . . . ?
C8 C13 C14 O16 -174.5(2) . . . . ?
C12 C13 C14 C15 -175.6(2) . . . . ?
C8 C13 C14 C15 6.7(3) . . . . ?
O16 C14 C15 C6 179.9(2) . . . . ?
C13 C14 C15 C6 -1.4(3) . . . . ?
O16 C14 C15 C2 -6.1(3) . . . . ?
C13 C14 C15 C2 172.5(2) . . . . ?
C5 C6 C15 C14 171.7(2) . . . . ?
C7 C6 C15 C14 -6.7(3) . . . . ?
C5 C6 C15 C2 -2.6(3) . . . . ?
C7 C6 C15 C2 179.1(2) . . . . ?
N1 C2 C15 C14 9.8(3) . . . . ?
C3 C2 C15 C14 -168.3(2) . . . . ?
N1 C2 C15 C6 -176.1(2) . . . . ?
C3 C2 C15 C6 5.8(3) . . . . ?
C36 C31 C32 C33 -1.9(4) . . . . ?
P30 C31 C32 C33 175.4(3) . . . . ?
C31 C32 C33 C34 0.9(5) . . . . ?
C32 C33 C34 C35 0.6(5) . . . . ?
C33 C34 C35 C36 -1.1(4) . . . . ?
C34 C35 C36 C31 0.0(4) . . . . ?
C32 C31 C36 C35 1.5(4) . . . . ?
P30 C31 C36 C35 -175.8(2) . . . . ?
C46 C41 C42 C43 -2.0(4) . . . . ?
P30 C41 C42 C43 178.6(2) . . . . ?
C41 C42 C43 C44 1.0(5) . . . . ?
C42 C43 C44 C45 0.2(6) . . . . ?
C43 C44 C45 C46 -0.3(6) . . . . ?
C42 C41 C46 C45 1.9(5) . . . . ?
P30 C41 C46 C45 -178.8(3) . . . . ?
C44 C45 C46 C41 -0.8(6) . . . . ?
C56 C51 C52 C53 -2.2(4) . . . . ?
P30 C51 C52 C53 -175.9(2) . . . . ?
C51 C52 C53 C54 1.0(4) . . . . ?
C52 C53 C54 C55 0.5(5) . . . . ?
C53 C54 C55 C56 -0.8(5) . . . . ?
C52 C51 C56 C55 1.9(4) . . . . ?
P30 C51 C56 C55 175.2(2) . . . . ?
C54 C55 C56 C51 -0.4(5) . . . . ?
C66 C61 C62 C63 -0.7(4) . . . . ?
P60 C61 C62 C63 -178.1(2) . . . . ?
C61 C62 C63 C64 1.2(5) . . . . ?
C62 C63 C64 C65 -0.5(5) . . . . ?
C63 C64 C65 C66 -0.8(5) . . . . ?
C62 C61 C66 C65 -0.6(4) . . . . ?
P60 C61 C66 C65 176.9(2) . . . . ?
C64 C65 C66 C61 1.4(5) . . . . ?
C76 C71 C72 C73 -0.8(4) . . . . ?
P60 C71 C72 C73 179.29(19) . . . . ?
C71 C72 C73 C74 0.4(4) . . . . ?
C72 C73 C74 C75 0.7(5) . . . . ?
C73 C74 C75 C76 -1.3(6) . . . . ?
C72 C71 C76 C75 0.2(5) . . . . ?
P60 C71 C76 C75 -179.9(3) . . . . ?
C74 C75 C76 C71 0.9(6) . . . . ?
C86 C81 C82 C83 0.1(4) . . . . ?
P60 C81 C82 C83 -171.7(2) . . . . ?
C81 C82 C83 C84 0.0(4) . . . . ?
C82 C83 C84 C85 -0.1(5) . . . . ?
C83 C84 C85 C86 0.2(5) . . . . ?
C82 C81 C86 C85 0.0(4) . . . . ?
P60 C81 C86 C85 171.5(2) . . . . ?
C84 C85 C86 C81 -0.1(4) . . . . ?
C3 C2 N1 Ru1 -174.23(16) . . . . ?
C15 C2 N1 Ru1 7.6(3) . . . . ?
C15 C14 O16 Ru1 -14.8(3) . . . . ?
C13 C14 O16 Ru1 166.53(14) . . . . ?
C56 C51 P30 C41 18.5(2) . . . . ?
C52 C51 P30 C41 -168.12(18) . . . . ?
C56 C51 P30 C31 123.8(2) . . . . ?
C52 C51 P30 C31 -62.8(2) . . . . ?
C56 C51 P30 Ru1 -110.7(2) . . . . ?
C52 C51 P30 Ru1 62.70(19) . . . . ?
C42 C41 P30 C51 -129.2(2) . . . . ?
C46 C41 P30 C51 51.5(3) . . . . ?
C42 C41 P30 C31 123.2(2) . . . . ?
C46 C41 P30 C31 -56.2(3) . . . . ?
C42 C41 P30 Ru1 -6.1(2) . . . . ?
C46 C41 P30 Ru1 174.6(2) . . . . ?
C36 C31 P30 C51 -1.3(2) . . . . ?
C32 C31 P30 C51 -178.5(2) . . . . ?
C36 C31 P30 C41 107.3(2) . . . . ?
C32 C31 P30 C41 -69.9(2) . . . . ?
C36 C31 P30 Ru1 -121.86(19) . . . . ?
C32 C31 P30 Ru1 60.9(2) . . . . ?
C86 C81 P60 C71 26.2(2) . . . . ?
C82 C81 P60 C71 -162.5(2) . . . . ?
C86 C81 P60 C61 132.8(2) . . . . ?
C82 C81 P60 C61 -55.8(2) . . . . ?
C86 C81 P60 Ru1 -103.8(2) . . . . ?
C82 C81 P60 Ru1 67.5(2) . . . . ?
C76 C71 P60 C81 61.1(3) . . . . ?
C72 C71 P60 C81 -119.0(2) . . . . ?
C76 C71 P60 C61 -47.6(3) . . . . ?
C72 C71 P60 C61 132.4(2) . . . . ?
C76 C71 P60 Ru1 -174.5(2) . . . . ?
C72 C71 P60 Ru1 5.4(2) . . . . ?
C66 C61 P60 C81 171.52(19) . . . . ?
C62 C61 P60 C81 -11.1(3) . . . . ?
C66 C61 P60 C71 -79.8(2) . . . . ?
C62 C61 P60 C71 97.7(2) . . . . ?
C66 C61 P60 Ru1 50.6(2) . . . . ?
C62 C61 P60 Ru1 -131.9(2) . . . . ?

_refine_diff_density_max         0.480
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.059

_shelxl_version_number           2014/6

