# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_xstr0803
_database_code_depnum_ccdc_archive 'CCDC 2009586'
loop_
_audit_author_name
_audit_author_address
'Derek A. Tocher'
;University College London
United Kingdom
;
_audit_update_record             
;
2020-06-13 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_audit_creation_date             2018-01-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C17 H6 N O10 Os3'
_chemical_formula_sum            'C17 H6 N O10 Os3'
_chemical_formula_weight         954.83
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Os3 C17 N1 O10 H7'
_chemical_oxdiff_usercomment     TR-06A
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7108(4)
_cell_length_b                   9.1324(4)
_cell_length_c                   14.1005(6)
_cell_angle_alpha                100.068(4)
_cell_angle_beta                 92.632(4)
_cell_angle_gamma                111.204(4)
_cell_volume                     1022.35(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9337
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      29.1180
_cell_measurement_theta_min      4.0880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.102
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15181
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.427
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     13.00  72.00   1.00    1.70    --   11.17  38.00   0.00   59
  2  ω     -3.00  87.00   1.00    1.70    --   11.17  77.00   0.00   90
  3  ω     -9.00  83.00   1.00    1.70    --   11.17  57.00 -90.00   92
  4  ω     -8.00  57.00   1.00    1.70    --   11.17-107.00  91.00   65
  5  ω    -20.00  52.00   1.00    1.70    --   11.17 -99.00 -30.00   72
  6  ω    -17.00  54.00   1.00    1.70    --   11.17-102.00-144.96   71
  7  ω    -84.00 -39.00   1.00    1.70    --  -10.07 -38.00 150.00   45
  8  ω    -13.00  85.00   1.00    1.70    --   11.17  38.00 150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0128328000
_diffrn_orient_matrix_UB_12      -0.0659363000
_diffrn_orient_matrix_UB_13      -0.0386527000
_diffrn_orient_matrix_UB_21      -0.0304152000
_diffrn_orient_matrix_UB_22      -0.0536837000
_diffrn_orient_matrix_UB_23      0.0316495000
_diffrn_orient_matrix_UB_31      -0.0815355000
_diffrn_orient_matrix_UB_32      -0.0041184000
_diffrn_orient_matrix_UB_33      -0.0123239000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3714
_reflns_number_total             4006
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         2.258
_refine_diff_density_min         -1.455
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       0.00091(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4006
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0269
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0641
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.17218(3) 0.63366(3) 0.81565(2) 0.01219(9) Uani 1 1 d . . . . .
Os2 Os 0.39717(3) 0.80451(3) 0.69870(2) 0.01143(9) Uani 1 1 d . . . . .
Os3 Os 0.70876(3) 0.98668(3) 0.63617(2) 0.01276(9) Uani 1 1 d . . . . .
O1 O -0.0992(6) 0.6264(6) 0.6695(4) 0.0286(12) Uani 1 1 d . . . . .
O2 O 0.1270(6) 0.9020(6) 0.9648(4) 0.0286(12) Uani 1 1 d . . . . .
O3 O -0.0531(6) 0.3484(6) 0.8909(4) 0.0309(12) Uani 1 1 d . . . . .
O4 O 0.2284(6) 1.0381(6) 0.6791(4) 0.0359(13) Uani 1 1 d . . . . .
O5 O 0.2818(6) 0.6554(6) 0.4823(3) 0.0277(11) Uani 1 1 d . . . . .
O6 O 0.5775(5) 1.0073(5) 0.8984(3) 0.0225(10) Uani 1 1 d . . . . .
O7 O 0.6342(6) 1.2787(6) 0.7348(4) 0.0312(12) Uani 1 1 d . . . . .
O8 O 0.9218(6) 0.9674(7) 0.8129(4) 0.0336(13) Uani 1 1 d . . . . .
O9 O 0.6557(6) 0.6570(6) 0.5090(4) 0.0267(11) Uani 1 1 d . . . . .
O10 O 0.9971(6) 1.1794(6) 0.5399(4) 0.0342(13) Uani 1 1 d . . . . .
N1 N 0.3940(6) 0.6463(6) 0.8951(4) 0.0126(11) Uani 1 1 d . . . . .
C1 C 0.0013(8) 0.6279(8) 0.7247(5) 0.0204(15) Uani 1 1 d . . . . .
C2 C 0.1410(7) 0.8026(8) 0.9113(5) 0.0165(14) Uani 1 1 d . . . . .
C3 C 0.0338(8) 0.4572(9) 0.8649(5) 0.0203(15) Uani 1 1 d . . . . .
C4 C 0.2942(8) 0.9513(8) 0.6855(5) 0.0187(14) Uani 1 1 d . . . . .
C5 C 0.3238(8) 0.7076(8) 0.5620(5) 0.0185(14) Uani 1 1 d . . . . .
C6 C 0.5079(8) 0.9301(7) 0.8261(5) 0.0161(14) Uani 1 1 d . . . . .
C7 C 0.6651(7) 1.1745(8) 0.7004(5) 0.0191(14) Uani 1 1 d . . . . .
C8 C 0.8428(8) 0.9737(8) 0.7493(5) 0.0199(15) Uani 1 1 d . . . . .
C9 C 0.6791(8) 0.7761(8) 0.5583(5) 0.0198(14) Uani 1 1 d . . . . .
C10 C 0.8917(8) 1.1066(8) 0.5761(5) 0.0242(16) Uani 1 1 d . . . . .
C11 C 0.2863(8) 0.5475(7) 0.7081(5) 0.0180(14) Uani 1 1 d . . . . .
H11 H 0.2241 0.4626 0.6521 0.022 Uiso 1 1 calc R . . . .
C12 C 0.4604(7) 0.5903(7) 0.7354(4) 0.0151(13) Uani 1 1 d . . . . .
H12 H 0.5228 0.5437 0.6918 0.018 Uiso 1 1 calc R . . . .
C13 C 0.5109(7) 0.6291(7) 0.8393(5) 0.0161(13) Uani 1 1 d . . . . .
C14 C 0.6673(7) 0.6519(8) 0.8831(5) 0.0200(15) Uani 1 1 d . . . . .
H14 H 0.7479 0.6396 0.8450 0.024 Uiso 1 1 calc R . . . .
C15 C 0.7014(8) 0.6921(8) 0.9811(5) 0.0224(15) Uani 1 1 d . . . . .
H15 H 0.8063 0.7093 1.0099 0.027 Uiso 1 1 calc R . . . .
C16 C 0.5816(8) 0.7079(8) 1.0386(5) 0.0210(15) Uani 1 1 d . . . . .
H16 H 0.6036 0.7346 1.1058 0.025 Uiso 1 1 calc R . . . .
C17 C 0.4291(8) 0.6827(7) 0.9927(5) 0.0178(14) Uani 1 1 d . . . . .
H17 H 0.3465 0.6911 1.0303 0.021 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os1 Os2 2.8248(4) . ?
Os1 N1 2.144(5) . ?
Os1 C1 1.899(7) . ?
Os1 C2 1.971(7) . ?
Os1 C3 1.896(7) . ?
Os1 C11 2.048(6) . ?
Os2 Os3 2.8945(4) . ?
Os2 C4 1.891(7) . ?
Os2 C5 1.946(7) . ?
Os2 C6 1.948(7) . ?
Os2 C11 2.223(6) . ?
Os2 C12 2.346(6) . ?
Os3 C7 1.966(7) . ?
Os3 C8 1.979(7) . ?
Os3 C9 1.961(7) . ?
Os3 C10 1.908(7) . ?
O1 C1 1.140(8) . ?
O2 C2 1.121(7) . ?
O3 C3 1.142(8) . ?
O4 C4 1.146(8) . ?
O5 C5 1.128(8) . ?
O6 C6 1.134(8) . ?
O7 C7 1.118(8) . ?
O8 C8 1.127(8) . ?
O9 C9 1.127(8) . ?
O10 C10 1.125(8) . ?
N1 C13 1.352(8) . ?
N1 C17 1.351(8) . ?
C11 C12 1.437(9) . ?
C12 C13 1.453(9) . ?
C13 C14 1.397(9) . ?
C14 C15 1.356(9) . ?
C15 C16 1.383(9) . ?
C16 C17 1.373(9) . ?

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 Os1 Os2 83.17(13) . . ?
C1 Os1 Os2 86.5(2) . . ?
C1 Os1 N1 168.7(2) . . ?
C1 Os1 C2 92.2(3) . . ?
C1 Os1 C3 94.5(3) . . ?
C1 Os1 C11 92.0(3) . . ?
C2 Os1 Os2 104.10(19) . . ?
C2 Os1 N1 94.6(2) . . ?
C2 Os1 C11 154.7(3) . . ?
C3 Os1 Os2 159.21(19) . . ?
C3 Os1 N1 93.6(2) . . ?
C3 Os1 C2 96.6(3) . . ?
C3 Os1 C11 107.9(3) . . ?
C11 Os1 Os2 51.31(17) . . ?
C11 Os1 N1 78.1(2) . . ?
Os1 Os2 Os3 159.593(12) . . ?
C4 Os2 Os1 96.3(2) . . ?
C4 Os2 Os3 96.0(2) . . ?
C4 Os2 C5 88.3(3) . . ?
C4 Os2 C6 90.9(3) . . ?
C4 Os2 C11 130.1(3) . . ?
C4 Os2 C12 164.3(2) . . ?
C5 Os2 Os1 110.54(18) . . ?
C5 Os2 Os3 86.08(18) . . ?
C5 Os2 C6 168.7(3) . . ?
C5 Os2 C11 80.2(3) . . ?
C5 Os2 C12 95.1(2) . . ?
C6 Os2 Os1 80.71(18) . . ?
C6 Os2 Os3 82.81(18) . . ?
C6 Os2 C11 108.6(2) . . ?
C6 Os2 C12 88.6(2) . . ?
C11 Os2 Os1 45.98(15) . . ?
C11 Os2 Os3 130.92(16) . . ?
C11 Os2 C12 36.5(2) . . ?
C12 Os2 Os1 68.21(14) . . ?
C12 Os2 Os3 99.51(15) . . ?
C7 Os3 Os2 84.35(18) . . ?
C7 Os3 C8 96.2(3) . . ?
C8 Os3 Os2 93.45(18) . . ?
C9 Os3 Os2 82.52(18) . . ?
C9 Os3 C7 162.3(3) . . ?
C9 Os3 C8 96.4(3) . . ?
C10 Os3 Os2 170.3(2) . . ?
C10 Os3 C7 95.1(3) . . ?
C10 Os3 C8 96.2(3) . . ?
C10 Os3 C9 95.8(3) . . ?
C13 N1 Os1 114.4(4) . . ?
C17 N1 Os1 125.8(4) . . ?
C17 N1 C13 119.5(5) . . ?
O1 C1 Os1 178.8(6) . . ?
O2 C2 Os1 177.9(6) . . ?
O3 C3 Os1 177.2(6) . . ?
O4 C4 Os2 178.0(6) . . ?
O5 C5 Os2 178.1(6) . . ?
O6 C6 Os2 177.1(5) . . ?
O7 C7 Os3 177.2(6) . . ?
O8 C8 Os3 178.7(6) . . ?
O9 C9 Os3 175.4(6) . . ?
O10 C10 Os3 178.1(7) . . ?
Os1 C11 Os2 82.7(2) . . ?
C12 C11 Os1 113.1(4) . . ?
C12 C11 Os2 76.4(4) . . ?
C11 C12 Os2 67.1(3) . . ?
C11 C12 C13 114.9(5) . . ?
C13 C12 Os2 106.5(4) . . ?
N1 C13 C12 115.0(5) . . ?
N1 C13 C14 119.6(6) . . ?
C14 C13 C12 125.4(5) . . ?
C15 C14 C13 120.0(6) . . ?
C14 C15 C16 120.6(6) . . ?
C17 C16 C15 117.6(6) . . ?
N1 C17 C16 122.7(6) . . ?


_olex2_date_sample_data_collection 2018-01-19
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id xstr0803
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.462
_oxdiff_exptl_absorpt_empirical_full_min 0.488
####################################################################### 
# 
# 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_tr_06c4_0m
_database_code_depnum_ccdc_archive 'CCDC 2009588'
loop_
_audit_author_name
_audit_author_address
'Shishir Ghosh'
;Jahangirnagar University
Bangladesh
;
_audit_update_record             
;
2020-06-13 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_audit_creation_date             2019-08-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H5 N O11 Os3, C0.5 Cl'
_chemical_formula_sum            'C17.50 H5 Cl N O11 Os3'
_chemical_formula_weight         1011.27
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.575(4)
_cell_length_b                   8.329(2)
_cell_length_c                   30.267(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.45(3)
_cell_angle_gamma                90
_cell_volume                     4402.6(17)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    193(1)
_cell_measurement_theta_max      27.107
_cell_measurement_theta_min      2.327
_shelx_estimated_absorpt_T_max   0.549
_shelx_estimated_absorpt_T_min   0.227
_exptl_absorpt_coefficient_mu    17.455
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1128 before and 0.0552 after correction. The Ratio of minimum to maximum transmission is 0.5403. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.051
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3600
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.039
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            32329
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.241
_diffrn_reflns_theta_min         2.332
_diffrn_ambient_temperature      193(1)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4460
_reflns_number_total             4927
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.219
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       0.000149(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4927
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0261
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0151P)²+48.1783P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0551
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C18(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C17(H17), C16(H16), C15(H15)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.55929(2) 0.53743(3) 0.36238(2) 0.01792(7) Uani 1 1 d . . . . .
C18 C 0.7560(15) 0.319(2) 0.5249(6) 0.082(7) Uani 0.5 1 d . . P . .
Cl1 Cl 0.71005(14) 0.3901(3) 0.48028(11) 0.0779(8) Uani 1 1 d . . . . .
Os2 Os 0.63509(2) 0.82121(3) 0.33846(2) 0.01767(7) Uani 1 1 d . . . . .
Os3 Os 0.77260(2) 0.61430(3) 0.34782(2) 0.01877(7) Uani 1 1 d . . . . .
O10 O 0.7439(2) 0.8011(5) 0.42787(14) 0.0253(9) Uani 1 1 d . . . . .
O7 O 0.9202(2) 0.7162(6) 0.30893(16) 0.0351(11) Uani 1 1 d . . . . .
O5 O 0.5838(3) 0.8361(8) 0.23895(17) 0.0544(16) Uani 1 1 d . . . . .
O4 O 0.4803(2) 0.9344(5) 0.36108(17) 0.0347(11) Uani 1 1 d . . . . .
O11 O 0.8621(2) 0.8418(6) 0.41218(16) 0.0349(11) Uani 1 1 d . . . . .
C11 C 0.6719(3) 0.6117(7) 0.37787(17) 0.0154(11) Uani 1 1 d . . . . .
N1 N 0.5516(3) 0.6579(5) 0.42407(16) 0.0179(10) Uani 1 1 d . . . . .
O1 O 0.5527(3) 0.2141(5) 0.40782(17) 0.0403(12) Uani 1 1 d . . . . .
C12 C 0.6738(3) 0.7356(7) 0.40973(19) 0.0180(11) Uani 1 1 d . . . . .
O3 O 0.5782(3) 0.3821(10) 0.2741(2) 0.076(2) Uani 1 1 d . . . . .
O2 O 0.3863(2) 0.5813(6) 0.33337(18) 0.0414(13) Uani 1 1 d . . . . .
C5 C 0.6022(3) 0.8310(9) 0.2759(2) 0.0317(15) Uani 1 1 d . . . . .
C4 C 0.5378(3) 0.8867(7) 0.3525(2) 0.0210(12) Uani 1 1 d . . . . .
O6 O 0.7055(3) 1.1540(6) 0.3526(2) 0.0560(16) Uani 1 1 d . . . . .
C3 C 0.5726(3) 0.4399(9) 0.3073(2) 0.0343(16) Uani 1 1 d . . . . .
O9 O 0.7369(3) 0.3874(9) 0.2682(2) 0.070(2) Uani 1 1 d . . . . .
O8 O 0.8464(3) 0.3493(7) 0.4066(2) 0.0516(16) Uani 1 1 d . . . . .
C6 C 0.6812(3) 1.0293(8) 0.3457(2) 0.0296(14) Uani 1 1 d . . . . .
C14 C 0.6174(4) 0.8270(8) 0.4791(2) 0.0282(14) Uani 1 1 d . . . . .
H14 H 0.661784 0.887157 0.489475 0.034 Uiso 1 1 calc R . . . .
C13 C 0.6138(3) 0.7447(7) 0.43932(19) 0.0190(11) Uani 1 1 d . . . . .
C7 C 0.8654(3) 0.6763(7) 0.3224(2) 0.0259(13) Uani 1 1 d . . . . .
C2 C 0.4494(3) 0.5607(7) 0.3438(2) 0.0261(14) Uani 1 1 d . . . . .
C1 C 0.5528(3) 0.3369(8) 0.3913(2) 0.0259(13) Uani 1 1 d . . . . .
C9 C 0.7455(3) 0.4698(9) 0.2978(3) 0.0363(17) Uani 1 1 d . . . . .
C17 C 0.4920(3) 0.6514(7) 0.4482(2) 0.0251(13) Uani 1 1 d . . . . .
H17 H 0.448342 0.589207 0.437643 0.030 Uiso 1 1 calc R . . . .
C10 C 0.8026(3) 0.7741(7) 0.4006(2) 0.0230(13) Uani 1 1 d . . . . .
C8 C 0.8200(3) 0.4469(8) 0.3842(2) 0.0286(14) Uani 1 1 d . . . . .
C16 C 0.4926(3) 0.7322(8) 0.4876(2) 0.0289(14) Uani 1 1 d . . . . .
H16 H 0.449560 0.726906 0.503955 0.035 Uiso 1 1 calc R . . . .
C15 C 0.5556(4) 0.8209(8) 0.5036(2) 0.0326(15) Uani 1 1 d . . . . .
H15 H 0.556793 0.877086 0.530968 0.039 Uiso 1 1 calc R . . . .
H H 0.724(3) 0.766(6) 0.3127(17) 0.003(12) Uiso 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 Os2 2.8464(9) . ?
Os1 C11 2.076(5) . ?
Os1 N1 2.137(5) . ?
Os1 C3 1.892(7) . ?
Os1 C2 1.960(6) . ?
Os1 C1 1.896(7) . ?
C18 C18 1.89(4) 7_656 ?
C18 Cl1 1.85(2) 7_656 ?
C18 Cl1 1.61(2) . ?
Os2 Os3 2.9561(10) . ?
Os2 C11 2.171(5) . ?
Os2 C12 2.301(6) . ?
Os2 C5 1.920(7) . ?
Os2 C4 1.889(6) . ?
Os2 C6 1.916(7) . ?
Os2 H 1.88(5) . ?
Os3 C11 2.079(5) . ?
Os3 C7 1.949(6) . ?
Os3 C9 1.950(8) . ?
Os3 C10 2.101(6) . ?
Os3 C8 1.908(7) . ?
Os3 H 1.80(5) . ?
O10 C12 1.401(6) . ?
O10 C10 1.410(7) . ?
O7 C7 1.136(7) . ?
O5 C5 1.128(8) . ?
O4 C4 1.141(7) . ?
O11 C10 1.204(7) . ?
C11 C12 1.410(8) . ?
N1 C13 1.349(7) . ?
N1 C17 1.344(7) . ?
O1 C1 1.137(8) . ?
C12 C13 1.460(8) . ?
O3 C3 1.128(8) . ?
O2 C2 1.131(7) . ?
O6 C6 1.133(8) . ?
O9 C9 1.126(9) . ?
O8 C8 1.125(8) . ?
C14 H14 0.9500 . ?
C14 C13 1.380(8) . ?
C14 C15 1.383(9) . ?
C17 H17 0.9500 . ?
C17 C16 1.370(9) . ?
C16 H16 0.9500 . ?
C16 C15 1.373(9) . ?
C15 H15 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 Os1 Os2 49.34(15) . . ?
C11 Os1 N1 79.35(19) . . ?
N1 Os1 Os2 84.82(13) . . ?
C3 Os1 Os2 91.4(2) . . ?
C3 Os1 C11 96.8(2) . . ?
C3 Os1 N1 175.8(2) . . ?
C3 Os1 C2 90.3(3) . . ?
C3 Os1 C1 92.8(3) . . ?
C2 Os1 Os2 108.62(18) . . ?
C2 Os1 C11 156.8(2) . . ?
C2 Os1 N1 92.7(2) . . ?
C1 Os1 Os2 154.62(18) . . ?
C1 Os1 C11 105.3(2) . . ?
C1 Os1 N1 89.8(2) . . ?
C1 Os1 C2 96.4(3) . . ?
Cl1 C18 C18 63.5(11) . 7_656 ?
Cl1 C18 C18 50.9(11) 7_656 7_656 ?
Cl1 C18 Cl1 114.3(11) . 7_656 ?
C18 Cl1 C18 65.7(11) . 7_656 ?
Os1 Os2 Os3 83.83(2) . . ?
Os1 Os2 H 109.6(15) . . ?
Os3 Os2 H 35.7(15) . . ?
C11 Os2 Os1 46.51(14) . . ?
C11 Os2 Os3 44.67(14) . . ?
C11 Os2 C12 36.6(2) . . ?
C11 Os2 H 79.6(15) . . ?
C12 Os2 Os1 66.55(14) . . ?
C12 Os2 Os3 64.97(14) . . ?
C12 Os2 H 98.0(15) . . ?
C5 Os2 Os1 100.9(2) . . ?
C5 Os2 Os3 105.76(19) . . ?
C5 Os2 C11 127.9(3) . . ?
C5 Os2 C12 164.4(3) . . ?
C5 Os2 H 76.9(15) . . ?
C4 Os2 Os1 73.80(18) . . ?
C4 Os2 Os3 153.90(18) . . ?
C4 Os2 C11 109.2(2) . . ?
C4 Os2 C12 93.3(2) . . ?
C4 Os2 C5 91.8(3) . . ?
C4 Os2 C6 95.5(3) . . ?
C4 Os2 H 168.6(15) . . ?
C6 Os2 Os1 157.9(2) . . ?
C6 Os2 Os3 100.69(18) . . ?
C6 Os2 C11 124.6(2) . . ?
C6 Os2 C12 95.5(2) . . ?
C6 Os2 C5 98.7(3) . . ?
C6 Os2 H 84.8(15) . . ?
Os2 Os3 H 37.6(15) . . ?
C11 Os3 Os2 47.22(15) . . ?
C11 Os3 C10 80.1(2) . . ?
C11 Os3 H 84.0(15) . . ?
C7 Os3 Os2 121.28(17) . . ?
C7 Os3 C11 165.1(2) . . ?
C7 Os3 C9 90.0(3) . . ?
C7 Os3 C10 89.0(2) . . ?
C7 Os3 H 86.8(15) . . ?
C9 Os3 Os2 99.2(2) . . ?
C9 Os3 C11 100.8(2) . . ?
C9 Os3 C10 178.6(3) . . ?
C9 Os3 H 85.2(16) . . ?
C10 Os3 Os2 80.57(15) . . ?
C10 Os3 H 93.8(16) . . ?
C8 Os3 Os2 141.29(17) . . ?
C8 Os3 C11 94.5(2) . . ?
C8 Os3 C7 95.2(2) . . ?
C8 Os3 C9 92.8(3) . . ?
C8 Os3 C10 88.2(3) . . ?
C8 Os3 H 177.2(16) . . ?
C12 O10 C10 112.2(4) . . ?
Os1 C11 Os2 84.14(18) . . ?
Os1 C11 Os3 137.8(3) . . ?
Os3 C11 Os2 88.1(2) . . ?
C12 C11 Os1 108.8(4) . . ?
C12 C11 Os2 76.7(3) . . ?
C12 C11 Os3 109.6(4) . . ?
C13 N1 Os1 114.9(4) . . ?
C17 N1 Os1 125.8(4) . . ?
C17 N1 C13 119.2(5) . . ?
O10 C12 Os2 113.7(4) . . ?
O10 C12 C11 120.4(5) . . ?
O10 C12 C13 113.8(5) . . ?
C11 C12 Os2 66.7(3) . . ?
C11 C12 C13 119.6(5) . . ?
C13 C12 Os2 113.6(4) . . ?
O5 C5 Os2 179.2(6) . . ?
O4 C4 Os2 176.4(5) . . ?
O3 C3 Os1 177.9(6) . . ?
O6 C6 Os2 174.9(6) . . ?
C13 C14 H14 120.4 . . ?
C13 C14 C15 119.2(6) . . ?
C15 C14 H14 120.4 . . ?
N1 C13 C12 112.1(5) . . ?
N1 C13 C14 121.4(5) . . ?
C14 C13 C12 126.5(5) . . ?
O7 C7 Os3 177.4(6) . . ?
O2 C2 Os1 176.9(6) . . ?
O1 C1 Os1 176.1(6) . . ?
O9 C9 Os3 173.5(6) . . ?
N1 C17 H17 119.2 . . ?
N1 C17 C16 121.5(6) . . ?
C16 C17 H17 119.2 . . ?
O10 C10 Os3 114.1(4) . . ?
O11 C10 Os3 130.8(5) . . ?
O11 C10 O10 115.0(6) . . ?
O8 C8 Os3 177.8(6) . . ?
C17 C16 H16 120.1 . . ?
C17 C16 C15 119.9(6) . . ?
C15 C16 H16 120.1 . . ?
C14 C15 H15 120.6 . . ?
C16 C15 C14 118.8(6) . . ?
C16 C15 H15 120.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_tr_63b_0m
_database_code_depnum_ccdc_archive 'CCDC 2009591'
loop_
_audit_author_name
_audit_author_address
'Shishir Ghosh'
;Jahangirnagar University
Bangladesh
;
_audit_update_record             
;
2020-06-13 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_audit_creation_date             2019-07-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H10 N2 O8 Ru3'
_chemical_formula_sum            'C22 H10 N2 O8 Ru3'
_chemical_formula_weight         733.53
_chemical_melting_point          ?
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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.187(5)
_cell_length_b                   9.641(6)
_cell_length_c                   15.139(9)
_cell_angle_alpha                97.65(3)
_cell_angle_beta                 94.716(17)
_cell_angle_gamma                106.30(2)
_cell_volume                     1127.7(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    193(1)
_cell_measurement_theta_max      27.094
_cell_measurement_theta_min      2.228
_shelx_estimated_absorpt_T_max   0.940
_shelx_estimated_absorpt_T_min   0.798
_exptl_absorpt_coefficient_mu    2.036
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0706 before and 0.0544 after correction. The Ratio of minimum to maximum transmission is 0.8830. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.031
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32047
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.155
_diffrn_reflns_theta_min         2.231
_diffrn_ambient_temperature      193(1)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-III CCD diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4049
_reflns_number_total             5010
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5010
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0323
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0491P)²+0.7111P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0854
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.77708(4) 0.74776(3) 0.84665(2) 0.02231(10) Uani 1 1 d . . . . .
O1 O 0.5521(5) 0.9392(4) 0.8989(3) 0.0543(10) Uani 1 1 d . . . . .
N1 N 0.5921(4) 0.3791(3) 0.8066(2) 0.0243(7) Uani 1 1 d . . . . .
C1 C 0.6385(6) 0.8693(5) 0.8821(3) 0.0348(10) Uani 1 1 d . . . . .
Ru2 Ru 0.84632(4) 0.62744(3) 0.68125(2) 0.02047(9) Uani 1 1 d . . . . .
O2 O 1.1275(4) 0.9514(4) 0.9345(2) 0.0425(8) Uani 1 1 d . . . . .
N2 N 0.5645(5) 0.7635(4) 0.5057(2) 0.0351(9) Uani 1 1 d . . . . .
C2 C 0.9958(6) 0.8759(5) 0.9061(3) 0.0293(9) Uani 1 1 d . . . . .
Ru3 Ru 0.86453(4) 0.48113(3) 0.83366(2) 0.02308(10) Uani 1 1 d . . . . .
O3 O 0.6856(5) 0.5978(4) 1.0108(2) 0.0457(9) Uani 1 1 d . . . . .
C3 C 0.7252(5) 0.6420(4) 0.9482(3) 0.0277(9) Uani 1 1 d . . . . .
C4 C 0.8255(5) 0.5484(5) 0.5577(3) 0.0310(10) Uani 1 1 d . . . . .
O4 O 0.8135(4) 0.5026(4) 0.4840(2) 0.0490(9) Uani 1 1 d . . . . .
O5 O 1.2297(4) 0.7646(4) 0.6951(2) 0.0488(9) Uani 1 1 d . . . . .
C5 C 1.0865(6) 0.7106(4) 0.6891(3) 0.0289(9) Uani 1 1 d . . . . .
C6 C 1.0988(6) 0.5813(5) 0.8675(3) 0.0291(9) Uani 1 1 d . . . . .
O6 O 1.2390(4) 0.6417(4) 0.8887(2) 0.0440(8) Uani 1 1 d . . . . .
C7 C 0.9008(5) 0.3203(5) 0.8789(3) 0.0331(10) Uani 1 1 d . . . . .
O7 O 0.9280(4) 0.2213(4) 0.9032(3) 0.0506(9) Uani 1 1 d . . . . .
C8 C 0.8904(5) 0.4270(4) 0.7059(3) 0.0226(8) Uani 1 1 d . . . . .
O8 O 0.9196(4) 0.3314(3) 0.6609(2) 0.0327(7) Uani 1 1 d . . . . .
C9 C 0.6013(5) 0.5968(4) 0.7475(3) 0.0229(8) Uani 1 1 d . . . . .
C10 C 0.5769(5) 0.6411(4) 0.6649(3) 0.0222(8) Uani 1 1 d . . . . .
H10 H 0.489273 0.580284 0.615364 0.027 Uiso 1 1 calc R . . . .
C11 C 0.6928(5) 0.7819(4) 0.6566(3) 0.0234(8) Uani 1 1 d . . . . .
C12 C 0.8124(5) 0.8442(4) 0.7330(3) 0.0244(8) Uani 1 1 d . . . . .
H12 H 0.904982 0.936392 0.734142 0.029 Uiso 1 1 calc R . . . .
C13 C 0.6811(5) 0.8452(4) 0.5727(3) 0.0246(8) Uani 1 1 d . . . . .
C14 C 0.7830(6) 0.9848(5) 0.5670(3) 0.0421(12) Uani 1 1 d . . . . .
H14 H 0.864637 1.040238 0.615370 0.050 Uiso 1 1 calc R . . . .
C15 C 0.7622(7) 1.0405(5) 0.4891(3) 0.0463(13) Uani 1 1 d . . . . .
H15 H 0.831516 1.133828 0.483010 0.056 Uiso 1 1 calc R . . . .
C16 C 0.6401(7) 0.9590(5) 0.4209(3) 0.0405(12) Uani 1 1 d . . . . .
H16 H 0.620778 0.995980 0.367891 0.049 Uiso 1 1 calc R . . . .
C17 C 0.5457(7) 0.8210(5) 0.4317(3) 0.0416(12) Uani 1 1 d . . . . .
H17 H 0.463230 0.764100 0.384088 0.050 Uiso 1 1 calc R . . . .
C18 C 0.5015(5) 0.4522(4) 0.7623(2) 0.0219(8) Uani 1 1 d . . . . .
C19 C 0.3270(5) 0.3924(4) 0.7372(3) 0.0275(9) Uani 1 1 d . . . . .
H19 H 0.265933 0.443483 0.705615 0.033 Uiso 1 1 calc R . . . .
C20 C 0.2426(5) 0.2594(5) 0.7582(3) 0.0326(10) Uani 1 1 d . . . . .
H20 H 0.123702 0.218639 0.741661 0.039 Uiso 1 1 calc R . . . .
C21 C 0.3359(6) 0.1861(5) 0.8041(3) 0.0352(10) Uani 1 1 d . . . . .
H21 H 0.281136 0.094607 0.819574 0.042 Uiso 1 1 calc R . . . .
C22 C 0.5077(6) 0.2481(4) 0.8267(3) 0.0302(9) Uani 1 1 d . . . . .
H22 H 0.570225 0.197233 0.857547 0.036 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C1 1.904(5) . ?
Ru1 Ru2 2.7868(15) . ?
Ru1 C2 1.933(5) . ?
Ru1 Ru3 2.8426(16) . ?
Ru1 C3 1.966(4) . ?
Ru1 C9 2.081(4) . ?
Ru1 C12 2.066(4) . ?
O1 C1 1.128(5) . ?
N1 Ru3 2.150(4) . ?
N1 C18 1.355(5) . ?
N1 C22 1.346(5) . ?
Ru2 Ru3 2.8747(15) . ?
Ru2 C4 1.898(5) . ?
Ru2 C5 1.891(5) . ?
Ru2 C8 2.137(4) . ?
Ru2 C9 2.279(4) . ?
Ru2 C10 2.241(4) . ?
Ru2 C11 2.250(4) . ?
Ru2 C12 2.233(4) . ?
O2 C2 1.130(5) . ?
N2 C13 1.329(5) . ?
N2 C17 1.330(6) . ?
Ru3 C6 1.882(5) . ?
Ru3 C7 1.863(5) . ?
Ru3 C8 1.980(4) . ?
O3 C3 1.124(5) . ?
C4 O4 1.131(5) . ?
O5 C5 1.131(5) . ?
C6 O6 1.128(5) . ?
C7 O7 1.138(5) . ?
C8 O8 1.163(5) . ?
C9 C10 1.391(5) . ?
C9 C18 1.461(5) . ?
C10 H10 0.9900 . ?
C10 C11 1.450(5) . ?
C11 C12 1.398(6) . ?
C11 C13 1.487(5) . ?
C12 H12 0.9900 . ?
C13 C14 1.389(6) . ?
C14 H14 0.9400 . ?
C14 C15 1.377(6) . ?
C15 H15 0.9400 . ?
C15 C16 1.362(7) . ?
C16 H16 0.9400 . ?
C16 C17 1.377(7) . ?
C17 H17 0.9400 . ?
C18 C19 1.381(6) . ?
C19 H19 0.9400 . ?
C19 C20 1.367(6) . ?
C20 H20 0.9400 . ?
C20 C21 1.383(6) . ?
C21 H21 0.9400 . ?
C21 C22 1.359(6) . ?
C22 H22 0.9400 . ?

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
C1 Ru1 Ru2 133.99(14) . . ?
C1 Ru1 C2 98.13(19) . . ?
C1 Ru1 Ru3 152.90(14) . . ?
C1 Ru1 C3 91.21(18) . . ?
C1 Ru1 C9 98.80(18) . . ?
C1 Ru1 C12 88.99(17) . . ?
Ru2 Ru1 Ru3 61.41(3) . . ?
C2 Ru1 Ru2 105.13(13) . . ?
C2 Ru1 Ru3 97.43(13) . . ?
C2 Ru1 C3 94.57(18) . . ?
C2 Ru1 C9 158.60(16) . . ?
C2 Ru1 C12 90.65(17) . . ?
C3 Ru1 Ru2 125.03(12) . . ?
C3 Ru1 Ru3 65.52(12) . . ?
C3 Ru1 C9 98.06(17) . . ?
C3 Ru1 C12 174.69(17) . . ?
C9 Ru1 Ru2 53.49(11) . . ?
C9 Ru1 Ru3 72.55(11) . . ?
C12 Ru1 Ru2 52.25(11) . . ?
C12 Ru1 Ru3 112.87(11) . . ?
C12 Ru1 C9 76.67(16) . . ?
C18 N1 Ru3 116.0(3) . . ?
C22 N1 Ru3 125.5(3) . . ?
C22 N1 C18 118.4(4) . . ?
O1 C1 Ru1 176.6(4) . . ?
Ru1 Ru2 Ru3 60.25(4) . . ?
C4 Ru2 Ru1 162.52(13) . . ?
C4 Ru2 Ru3 128.06(14) . . ?
C4 Ru2 C8 85.54(17) . . ?
C4 Ru2 C9 117.81(17) . . ?
C4 Ru2 C10 90.84(16) . . ?
C4 Ru2 C11 93.83(16) . . ?
C4 Ru2 C12 124.51(17) . . ?
C5 Ru2 Ru1 101.90(13) . . ?
C5 Ru2 Ru3 94.42(12) . . ?
C5 Ru2 C4 93.08(18) . . ?
C5 Ru2 C8 88.35(16) . . ?
C5 Ru2 C9 148.99(17) . . ?
C5 Ru2 C10 152.26(16) . . ?
C5 Ru2 C11 114.62(16) . . ?
C5 Ru2 C12 91.49(17) . . ?
C8 Ru2 Ru1 103.68(11) . . ?
C8 Ru2 Ru3 43.51(11) . . ?
C8 Ru2 C9 96.28(15) . . ?
C8 Ru2 C10 119.34(14) . . ?
C8 Ru2 C11 157.01(15) . . ?
C8 Ru2 C12 149.90(15) . . ?
C9 Ru2 Ru1 47.20(10) . . ?
C9 Ru2 Ru3 69.46(10) . . ?
C10 Ru2 Ru1 71.71(10) . . ?
C10 Ru2 Ru3 104.63(10) . . ?
C10 Ru2 C9 35.82(14) . . ?
C10 Ru2 C11 37.67(14) . . ?
C11 Ru2 Ru1 71.83(11) . . ?
C11 Ru2 Ru3 128.14(10) . . ?
C11 Ru2 C9 63.72(14) . . ?
C12 Ru2 Ru1 47.02(10) . . ?
C12 Ru2 Ru3 106.59(11) . . ?
C12 Ru2 C9 69.49(14) . . ?
C12 Ru2 C10 64.05(15) . . ?
C12 Ru2 C11 36.35(14) . . ?
C13 N2 C17 117.6(4) . . ?
O2 C2 Ru1 174.8(4) . . ?
Ru1 Ru3 Ru2 58.34(3) . . ?
N1 Ru3 Ru1 84.58(9) . . ?
N1 Ru3 Ru2 89.28(9) . . ?
C6 Ru3 Ru1 91.93(13) . . ?
C6 Ru3 N1 174.35(16) . . ?
C6 Ru3 Ru2 92.66(13) . . ?
C6 Ru3 C8 94.36(17) . . ?
C7 Ru3 Ru1 153.71(14) . . ?
C7 Ru3 N1 92.38(16) . . ?
C7 Ru3 Ru2 147.89(14) . . ?
C7 Ru3 C6 88.79(18) . . ?
C7 Ru3 C8 99.90(18) . . ?
C8 Ru3 Ru1 106.24(11) . . ?
C8 Ru3 N1 90.88(14) . . ?
C8 Ru3 Ru2 48.00(11) . . ?
O3 C3 Ru1 169.6(4) . . ?
O4 C4 Ru2 179.4(4) . . ?
O5 C5 Ru2 177.8(4) . . ?
O6 C6 Ru3 179.3(4) . . ?
O7 C7 Ru3 176.5(4) . . ?
Ru3 C8 Ru2 88.49(16) . . ?
O8 C8 Ru2 133.8(3) . . ?
O8 C8 Ru3 137.7(3) . . ?
Ru1 C9 Ru2 79.32(14) . . ?
C10 C9 Ru1 116.8(3) . . ?
C10 C9 Ru2 70.6(2) . . ?
C10 C9 C18 120.0(4) . . ?
C18 C9 Ru1 123.2(3) . . ?
C18 C9 Ru2 121.2(3) . . ?
Ru2 C10 H10 122.7 . . ?
C9 C10 Ru2 73.6(2) . . ?
C9 C10 H10 122.7 . . ?
C9 C10 C11 114.6(3) . . ?
C11 C10 Ru2 71.5(2) . . ?
C11 C10 H10 122.7 . . ?
C10 C11 Ru2 70.9(2) . . ?
C10 C11 C13 121.0(3) . . ?
C12 C11 Ru2 71.2(2) . . ?
C12 C11 C10 112.8(3) . . ?
C12 C11 C13 126.2(4) . . ?
C13 C11 Ru2 124.7(3) . . ?
Ru1 C12 Ru2 80.73(13) . . ?
Ru1 C12 H12 121.0 . . ?
Ru2 C12 H12 121.0 . . ?
C11 C12 Ru1 117.8(3) . . ?
C11 C12 Ru2 72.5(2) . . ?
C11 C12 H12 121.0 . . ?
N2 C13 C11 116.5(4) . . ?
N2 C13 C14 122.4(4) . . ?
C14 C13 C11 121.1(4) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 C13 118.7(4) . . ?
C15 C14 H14 120.6 . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.3(4) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 120.9 . . ?
C15 C16 C17 118.3(4) . . ?
C17 C16 H16 120.9 . . ?
N2 C17 C16 123.8(5) . . ?
N2 C17 H17 118.1 . . ?
C16 C17 H17 118.1 . . ?
N1 C18 C9 114.8(3) . . ?
N1 C18 C19 120.6(4) . . ?
C19 C18 C9 124.5(4) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.4(4) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 120.7 . . ?
C19 C20 C21 118.6(4) . . ?
C21 C20 H20 120.7 . . ?
C20 C21 H21 120.4 . . ?
C22 C21 C20 119.1(4) . . ?
C22 C21 H21 120.4 . . ?
N1 C22 C21 122.8(4) . . ?
N1 C22 H22 118.6 . . ?
C21 C22 H22 118.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_tr_63e_0m
_database_code_depnum_ccdc_archive 'CCDC 2009592'
loop_
_audit_author_name
_audit_author_address
'Shishir Ghosh'
;Jahangirnagar University
Bangladesh
;
_audit_update_record             
;
2020-06-13 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_audit_creation_date             2019-07-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H15 N3 O8 Ru3'
_chemical_formula_sum            'C29 H15 N3 O8 Ru3'
_chemical_formula_weight         836.65
_chemical_melting_point          ?
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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.114(18)
_cell_length_b                   11.221(17)
_cell_length_c                   13.16(2)
_cell_angle_alpha                75.91(5)
_cell_angle_beta                 73.55(6)
_cell_angle_gamma                61.99(9)
_cell_volume                     1377(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    193(1)
_cell_measurement_theta_max      27.083
_cell_measurement_theta_min      2.227
_shelx_estimated_absorpt_T_max   0.931
_shelx_estimated_absorpt_T_min   0.683
_exptl_absorpt_coefficient_mu    1.682
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1432 before and 0.0729 after correction. The Ratio of minimum to maximum transmission is 0.7599. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.043
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31001
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.218
_diffrn_reflns_theta_min         2.236
_diffrn_ambient_temperature      193(1)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX3 CCD diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4494
_reflns_number_total             6101
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         3.272
_refine_diff_density_min         -1.454
_refine_diff_density_rms         0.228
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0687
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0652P)²+26.0485P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1872
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C11(H11), C13(H13)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
 C24(H24), C26(H26), C27(H27), C28(H28), C29(H29)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.68856(7) 0.33997(7) 0.23399(6) 0.02481(19) Uani 1 1 d . . . . .
O1 O 0.9957(7) 0.1579(8) 0.2008(7) 0.0455(19) Uani 1 1 d . . . . .
N1 N 0.8781(10) -0.0790(9) 0.2467(8) 0.044(2) Uani 1 1 d . . . . .
C1 C 0.8861(10) 0.2463(10) 0.2117(7) 0.0298(19) Uani 1 1 d . . . . .
Ru2 Ru 0.47637(7) 0.25857(8) 0.29258(6) 0.0271(2) Uani 1 1 d . . . . .
O2 O 0.6728(8) 0.4106(9) -0.0029(6) 0.048(2) Uani 1 1 d . . . . .
N2 N 0.8383(8) 0.3443(9) 0.4187(6) 0.0340(18) Uani 1 1 d . . . . .
C2 C 0.6785(10) 0.3860(10) 0.0858(8) 0.035(2) Uani 1 1 d . . . . .
Ru3 Ru 0.82953(8) 0.47096(8) 0.26793(6) 0.0314(2) Uani 1 1 d . . . . .
O3 O 0.2097(8) 0.5157(10) 0.3402(9) 0.067(3) Uani 1 1 d . . . . .
N3 N 0.4079(11) 0.7033(11) 0.2151(8) 0.053(3) Uani 1 1 d . . . . .
C3 C 0.3110(11) 0.4229(10) 0.3212(10) 0.039(2) Uani 1 1 d . . . . .
C4 C 0.3735(10) 0.1559(10) 0.3542(9) 0.037(2) Uani 1 1 d . . . . .
O4 O 0.3115(9) 0.0948(9) 0.3941(8) 0.060(2) Uani 1 1 d . . . . .
C5 C 0.4567(10) 0.2672(10) 0.1517(8) 0.035(2) Uani 1 1 d . . . . .
O5 O 0.4458(8) 0.2689(10) 0.0659(6) 0.054(2) Uani 1 1 d . . . . .
C6 C 0.8227(11) 0.5696(13) 0.1304(10) 0.044(3) Uani 1 1 d . . . . .
O6 O 0.7915(10) 0.6903(10) 0.3869(8) 0.062(2) Uani 1 1 d . . . . .
C7 C 0.8052(12) 0.6143(13) 0.3361(9) 0.045(3) Uani 1 1 d . . . . .
O7 O 1.1493(8) 0.3364(11) 0.2015(8) 0.067(3) Uani 1 1 d . . . . .
C8 C 1.0341(11) 0.3855(12) 0.2293(8) 0.037(2) Uani 1 1 d . . . . .
O8 O 0.8175(10) 0.6295(10) 0.0461(7) 0.064(3) Uani 1 1 d . . . . .
C9 C 0.6990(9) 0.1438(9) 0.2639(7) 0.0256(18) Uani 1 1 d . . . . .
C10 C 0.6468(9) 0.1104(9) 0.3730(7) 0.0269(18) Uani 1 1 d . . . . .
H10 H 0.656122 0.016547 0.404271 0.032 Uiso 1 1 calc R . . . .
C12 C 0.6381(9) 0.3162(9) 0.4054(7) 0.0228(17) Uani 1 1 d . . . . .
C11 C 0.5721(10) 0.2231(10) 0.4330(8) 0.032(2) Uani 1 1 d . . . . .
H11 H 0.519664 0.211272 0.507335 0.038 Uiso 1 1 calc R . . . .
C14 C 0.6149(9) 0.5403(9) 0.2983(7) 0.0277(19) Uani 1 1 d . . . . .
C13 C 0.5528(9) 0.4616(9) 0.3719(7) 0.0277(19) Uani 1 1 d . . . . .
H13 H 0.449743 0.495196 0.383783 0.033 Uiso 1 1 calc R . . . .
C15 C 0.7900(9) 0.0327(9) 0.1972(8) 0.0276(19) Uani 1 1 d . . . . .
C16 C 0.7886(11) 0.0403(11) 0.0915(8) 0.041(2) Uani 1 1 d . . . . .
H16 H 0.725400 0.121108 0.057115 0.049 Uiso 1 1 calc R . . . .
C17 C 0.8778(12) -0.0677(12) 0.0349(9) 0.049(3) Uani 1 1 d . . . . .
H17 H 0.875595 -0.062813 -0.037702 0.058 Uiso 1 1 calc R . . . .
C18 C 0.9695(12) -0.1820(12) 0.0856(10) 0.048(3) Uani 1 1 d . . . . .
H18 H 1.033565 -0.258193 0.049112 0.057 Uiso 1 1 calc R . . . .
C19 C 0.9659(12) -0.1831(11) 0.1888(9) 0.047(3) Uani 1 1 d . . . . .
H19 H 1.029629 -0.262797 0.223729 0.056 Uiso 1 1 calc R . . . .
C20 C 0.7572(9) 0.2788(10) 0.4563(7) 0.0294(19) Uani 1 1 d . . . . .
C21 C 0.7868(11) 0.1720(11) 0.5410(8) 0.038(2) Uani 1 1 d . . . . .
H21 H 0.728777 0.125957 0.567543 0.045 Uiso 1 1 calc R . . . .
C22 C 0.8989(12) 0.1341(11) 0.5853(9) 0.044(3) Uani 1 1 d . . . . .
H22 H 0.919541 0.061087 0.641908 0.053 Uiso 1 1 calc R . . . .
C23 C 0.9821(11) 0.2024(12) 0.5474(9) 0.043(3) Uani 1 1 d . . . . .
H23 H 1.060868 0.177406 0.576710 0.052 Uiso 1 1 calc R . . . .
C24 C 0.9471(10) 0.3067(11) 0.4665(8) 0.038(2) Uani 1 1 d . . . . .
H24 H 1.001798 0.356310 0.441957 0.046 Uiso 1 1 calc R . . . .
C25 C 0.5245(11) 0.6791(11) 0.2515(9) 0.038(2) Uani 1 1 d . . . . .
C26 C 0.5633(11) 0.7761(10) 0.2437(10) 0.041(3) Uani 1 1 d . . . . .
H26 H 0.642872 0.757452 0.269461 0.050 Uiso 1 1 calc R . . . .
C27 C 0.4892(16) 0.8998(13) 0.1991(13) 0.066(4) Uani 1 1 d . . . . .
H27 H 0.518869 0.968642 0.192434 0.079 Uiso 1 1 calc R . . . .
C28 C 0.3713(13) 0.9342(13) 0.1618(10) 0.054(3) Uani 1 1 d . . . . .
H28 H 0.320687 1.024324 0.130527 0.065 Uiso 1 1 calc R . . . .
C29 C 0.3303(13) 0.8353(12) 0.1714(10) 0.050(3) Uani 1 1 d . . . . .
H29 H 0.248213 0.856043 0.148226 0.061 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 C1 1.905(10) . ?
Ru1 Ru2 2.764(4) . ?
Ru1 C2 1.913(11) . ?
Ru1 Ru3 2.774(3) . ?
Ru1 C9 2.093(10) . ?
Ru1 C12 2.146(9) . ?
Ru1 C14 2.291(9) . ?
Ru1 C13 2.270(9) . ?
O1 C1 1.150(12) . ?
N1 C15 1.328(12) . ?
N1 C19 1.357(14) . ?
C1 Ru3 2.541(10) . ?
Ru2 C3 1.919(11) . ?
Ru2 C4 1.884(11) . ?
Ru2 C5 1.902(11) . ?
Ru2 C9 2.154(9) . ?
Ru2 C10 2.189(9) . ?
Ru2 C11 2.249(10) . ?
O2 C2 1.144(12) . ?
N2 Ru3 2.138(9) . ?
N2 C20 1.338(13) . ?
N2 C24 1.363(12) . ?
Ru3 C6 1.879(13) . ?
Ru3 C7 1.903(12) . ?
Ru3 C8 1.970(11) . ?
Ru3 C14 2.079(10) . ?
O3 C3 1.132(13) . ?
N3 C25 1.393(14) . ?
N3 C29 1.391(15) . ?
C4 O4 1.133(13) . ?
C5 O5 1.163(12) . ?
C6 O8 1.149(14) . ?
O6 C7 1.138(14) . ?
O7 C8 1.117(13) . ?
C9 C10 1.417(13) . ?
C9 C15 1.481(13) . ?
C10 H10 1.0000 . ?
C10 C11 1.428(13) . ?
C12 C11 1.465(13) . ?
C12 C13 1.480(12) . ?
C12 C20 1.490(12) . ?
C11 H11 1.0000 . ?
C14 C13 1.405(14) . ?
C14 C25 1.493(14) . ?
C13 H13 1.0000 . ?
C15 C16 1.376(14) . ?
C16 H16 0.9500 . ?
C16 C17 1.378(15) . ?
C17 H17 0.9500 . ?
C17 C18 1.367(16) . ?
C18 H18 0.9500 . ?
C18 C19 1.344(16) . ?
C19 H19 0.9500 . ?
C20 C21 1.406(14) . ?
C21 H21 0.9500 . ?
C21 C22 1.365(15) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(17) . ?
C23 H23 0.9500 . ?
C23 C24 1.362(16) . ?
C24 H24 0.9500 . ?
C25 C26 1.320(15) . ?
C26 H26 0.9500 . ?
C26 C27 1.324(17) . ?
C27 H27 0.9500 . ?
C27 C28 1.379(19) . ?
C28 H28 0.9500 . ?
C28 C29 1.354(18) . ?
C29 H29 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ru1 Ru2 134.3(3) . . ?
C1 Ru1 C2 95.8(4) . . ?
C1 Ru1 Ru3 62.6(3) . . ?
C1 Ru1 C9 84.0(4) . . ?
C1 Ru1 C12 100.1(4) . . ?
C1 Ru1 C14 109.7(4) . . ?
C1 Ru1 C13 124.3(4) . . ?
Ru2 Ru1 Ru3 152.05(6) . . ?
C2 Ru1 Ru2 94.6(3) . . ?
C2 Ru1 Ru3 106.5(3) . . ?
C2 Ru1 C9 100.9(4) . . ?
C2 Ru1 C12 164.0(4) . . ?
C2 Ru1 C14 106.6(4) . . ?
C2 Ru1 C13 129.2(4) . . ?
C9 Ru1 Ru2 50.4(2) . . ?
C9 Ru1 Ru3 138.2(2) . . ?
C9 Ru1 C12 80.4(3) . . ?
C9 Ru1 C14 147.6(4) . . ?
C9 Ru1 C13 112.0(4) . . ?
C12 Ru1 Ru2 73.7(2) . . ?
C12 Ru1 Ru3 81.7(2) . . ?
C12 Ru1 C14 68.5(3) . . ?
C12 Ru1 C13 39.0(3) . . ?
C14 Ru1 Ru2 109.6(3) . . ?
C14 Ru1 Ru3 47.3(2) . . ?
C13 Ru1 Ru2 79.4(2) . . ?
C13 Ru1 Ru3 73.1(2) . . ?
C13 Ru1 C14 35.9(3) . . ?
C15 N1 C19 117.3(9) . . ?
Ru1 C1 Ru3 75.7(3) . . ?
O1 C1 Ru1 159.5(9) . . ?
O1 C1 Ru3 123.7(7) . . ?
C3 Ru2 Ru1 104.1(3) . . ?
C3 Ru2 C9 151.7(4) . . ?
C3 Ru2 C10 137.6(4) . . ?
C3 Ru2 C11 100.5(4) . . ?
C4 Ru2 Ru1 162.0(3) . . ?
C4 Ru2 C3 90.0(4) . . ?
C4 Ru2 C5 93.4(4) . . ?
C4 Ru2 C9 115.6(4) . . ?
C4 Ru2 C10 90.8(4) . . ?
C4 Ru2 C11 97.7(4) . . ?
C5 Ru2 Ru1 96.6(3) . . ?
C5 Ru2 C3 94.3(5) . . ?
C5 Ru2 C9 96.0(4) . . ?
C5 Ru2 C10 128.0(4) . . ?
C5 Ru2 C11 161.5(4) . . ?
C9 Ru2 Ru1 48.4(3) . . ?
C9 Ru2 C10 38.1(3) . . ?
C9 Ru2 C11 65.9(3) . . ?
C10 Ru2 Ru1 71.3(3) . . ?
C10 Ru2 C11 37.5(3) . . ?
C11 Ru2 Ru1 69.1(3) . . ?
C20 N2 Ru3 121.3(6) . . ?
C20 N2 C24 118.2(9) . . ?
C24 N2 Ru3 119.1(7) . . ?
O2 C2 Ru1 178.4(9) . . ?
C1 Ru3 Ru1 41.7(2) . . ?
N2 Ru3 Ru1 84.4(2) . . ?
N2 Ru3 C1 79.3(3) . . ?
C6 Ru3 Ru1 91.3(3) . . ?
C6 Ru3 C1 95.7(4) . . ?
C6 Ru3 N2 174.9(4) . . ?
C6 Ru3 C7 95.9(5) . . ?
C6 Ru3 C8 89.5(5) . . ?
C6 Ru3 C14 89.5(4) . . ?
C7 Ru3 Ru1 142.7(4) . . ?
C7 Ru3 C1 167.3(4) . . ?
C7 Ru3 N2 89.1(4) . . ?
C7 Ru3 C8 98.7(5) . . ?
C7 Ru3 C14 89.4(4) . . ?
C8 Ru3 Ru1 118.0(3) . . ?
C8 Ru3 C1 76.5(4) . . ?
C8 Ru3 N2 90.1(4) . . ?
C8 Ru3 C14 172.0(4) . . ?
C14 Ru3 Ru1 54.1(3) . . ?
C14 Ru3 C1 95.7(3) . . ?
C14 Ru3 N2 90.1(4) . . ?
C29 N3 C25 117.7(11) . . ?
O3 C3 Ru2 176.4(10) . . ?
O4 C4 Ru2 178.1(10) . . ?
O5 C5 Ru2 178.2(9) . . ?
O8 C6 Ru3 179.3(10) . . ?
O6 C7 Ru3 172.5(11) . . ?
O7 C8 Ru3 175.7(9) . . ?
Ru1 C9 Ru2 81.2(3) . . ?
C10 C9 Ru1 111.3(6) . . ?
C10 C9 Ru2 72.3(5) . . ?
C10 C9 C15 119.0(8) . . ?
C15 C9 Ru1 126.4(6) . . ?
C15 C9 Ru2 129.9(6) . . ?
Ru2 C10 H10 122.6 . . ?
C9 C10 Ru2 69.6(5) . . ?
C9 C10 H10 122.6 . . ?
C9 C10 C11 114.7(8) . . ?
C11 C10 Ru2 73.5(5) . . ?
C11 C10 H10 122.6 . . ?
C11 C12 Ru1 103.9(6) . . ?
C11 C12 C13 118.0(8) . . ?
C11 C12 C20 117.4(8) . . ?
C13 C12 Ru1 75.0(5) . . ?
C13 C12 C20 118.9(8) . . ?
C20 C12 Ru1 113.8(6) . . ?
Ru2 C11 H11 119.8 . . ?
C10 C11 Ru2 68.9(5) . . ?
C10 C11 C12 112.2(8) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 Ru2 105.1(6) . . ?
C12 C11 H11 119.8 . . ?
Ru3 C14 Ru1 78.6(3) . . ?
C13 C14 Ru1 71.3(5) . . ?
C13 C14 Ru3 119.7(7) . . ?
C13 C14 C25 119.2(8) . . ?
C25 C14 Ru1 126.4(6) . . ?
C25 C14 Ru3 120.8(7) . . ?
Ru1 C13 H13 118.6 . . ?
C12 C13 Ru1 65.9(4) . . ?
C12 C13 H13 118.6 . . ?
C14 C13 Ru1 72.9(5) . . ?
C14 C13 C12 120.2(8) . . ?
C14 C13 H13 118.6 . . ?
N1 C15 C9 114.8(9) . . ?
N1 C15 C16 120.6(9) . . ?
C16 C15 C9 124.6(8) . . ?
C15 C16 H16 119.6 . . ?
C15 C16 C17 120.9(10) . . ?
C17 C16 H16 119.6 . . ?
C16 C17 H17 120.8 . . ?
C18 C17 C16 118.5(10) . . ?
C18 C17 H17 120.8 . . ?
C17 C18 H18 121.1 . . ?
C19 C18 C17 117.8(10) . . ?
C19 C18 H18 121.1 . . ?
N1 C19 H19 117.5 . . ?
C18 C19 N1 124.9(10) . . ?
C18 C19 H19 117.5 . . ?
N2 C20 C12 119.8(8) . . ?
N2 C20 C21 120.2(9) . . ?
C21 C20 C12 120.0(9) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.2(11) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 120.1 . . ?
C21 C22 C23 119.8(10) . . ?
C23 C22 H22 120.1 . . ?
C22 C23 H23 121.2 . . ?
C24 C23 C22 117.6(10) . . ?
C24 C23 H23 121.2 . . ?
N2 C24 H24 118.0 . . ?
C23 C24 N2 123.9(11) . . ?
C23 C24 H24 118.0 . . ?
N3 C25 C14 121.4(10) . . ?
C26 C25 N3 122.1(10) . . ?
C26 C25 C14 116.4(9) . . ?
C25 C26 H26 120.7 . . ?
C25 C26 C27 118.7(11) . . ?
C27 C26 H26 120.7 . . ?
C26 C27 H27 118.2 . . ?
C26 C27 C28 123.6(13) . . ?
C28 C27 H27 118.2 . . ?
C27 C28 H28 121.1 . . ?
C29 C28 C27 117.7(12) . . ?
C29 C28 H28 121.1 . . ?
N3 C29 H29 119.9 . . ?
C28 C29 N3 120.2(12) . . ?
C28 C29 H29 119.9 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_xstr0818
_database_code_depnum_ccdc_archive 'CCDC 2009587'
loop_
_audit_author_name
_audit_author_address
'Derek A. Tocher'
;University College London
United Kingdom
;
_audit_update_record             
;
2020-06-13 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_audit_creation_date             2019-07-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H6 N O9 Os3'
_chemical_formula_sum            'C16 H6 N O9 Os3'
_chemical_formula_weight         926.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Os3 O9 N1 C16 H7'
_chemical_oxdiff_usercomment     PM-8A
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.1249(2)
_cell_length_b                   15.2910(4)
_cell_length_c                   15.3121(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.697(2)
_cell_angle_gamma                90
_cell_volume                     1901.52(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16199
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      29.2840
_cell_measurement_theta_min      3.8680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.047
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.237
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30729
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         3.168
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -13.00  85.00   1.00    2.42    --   11.17  38.00 -60.00   98
  2  ω    -14.00  84.00   1.00    2.42    --   11.17  57.00  30.00   98
  3  ω    -15.00  87.00   1.00    2.42    --   11.17  77.00 150.00  102
  4  ω    -19.00  52.00   1.00    2.42    --   11.17 -99.00   0.00   71
  5  ω     38.00  91.00   1.00    2.42    --   11.17-178.00 -90.00   53
  6  ω    -18.00  52.00   1.00    2.42    --   11.17 -99.00 120.00   70
  7  ω    -54.00  39.00   1.00    2.42    --   11.17 -57.00-120.00   93
  8  ω    -86.00 -61.00   1.00    2.42    --  -10.07 154.00  90.29   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0475379000
_diffrn_orient_matrix_UB_12      0.0251358000
_diffrn_orient_matrix_UB_13      -0.0304272000
_diffrn_orient_matrix_UB_21      0.0154812000
_diffrn_orient_matrix_UB_22      0.0380884000
_diffrn_orient_matrix_UB_23      0.0253769000
_diffrn_orient_matrix_UB_31      0.0716159000
_diffrn_orient_matrix_UB_32      0.0084616000
_diffrn_orient_matrix_UB_33      -0.0239872000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3857
_reflns_number_total             4142
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.062
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4142
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0211
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0168P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0471
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.13888(2) 0.76243(2) 0.18649(2) 0.01120(6) Uani 1 1 d . . . . .
Os2 Os -0.13738(2) 0.64693(2) 0.17476(2) 0.01073(6) Uani 1 1 d . . . . .
Os3 Os 0.08448(2) 0.66464(2) 0.03443(2) 0.01156(6) Uani 1 1 d . . . . .
O1 O 0.0601(5) 0.8235(3) 0.3707(2) 0.0305(9) Uani 1 1 d . . . . .
O2 O 0.4305(4) 0.8786(3) 0.1448(3) 0.0315(9) Uani 1 1 d . . . . .
O3 O 0.3751(4) 0.6216(3) 0.2507(3) 0.0297(9) Uani 1 1 d . . . . .
O4 O -0.3541(4) 0.4833(3) 0.1712(3) 0.0287(9) Uani 1 1 d . . . . .
O5 O -0.3412(5) 0.7722(3) 0.2819(2) 0.0322(10) Uani 1 1 d . . . . .
O6 O 0.0423(4) 0.5742(2) 0.3371(2) 0.0271(9) Uani 1 1 d . . . . .
O7 O 0.3749(4) 0.5377(3) 0.0522(3) 0.0342(10) Uani 1 1 d . . . . .
O8 O 0.2871(4) 0.8082(2) -0.0462(2) 0.0264(8) Uani 1 1 d . . . . .
O9 O -0.0618(4) 0.5887(2) -0.1352(2) 0.0242(8) Uani 1 1 d . . . . .
N1 N -0.0216(4) 0.8587(3) 0.1252(2) 0.0122(8) Uani 1 1 d . . . . .
C1 C 0.0881(5) 0.8031(3) 0.3012(3) 0.0168(10) Uani 1 1 d . . . . .
C2 C 0.3210(6) 0.8347(3) 0.1609(3) 0.0199(11) Uani 1 1 d . . . . .
C3 C 0.2832(5) 0.6744(3) 0.2262(3) 0.0158(10) Uani 1 1 d . . . . .
C4 C -0.2792(5) 0.5452(3) 0.1699(3) 0.0171(11) Uani 1 1 d . . . . .
C5 C -0.2637(6) 0.7237(3) 0.2442(3) 0.0179(11) Uani 1 1 d . . . . .
C6 C -0.0208(6) 0.6026(3) 0.2755(3) 0.0166(10) Uani 1 1 d . . . . .
C7 C 0.2708(6) 0.5868(3) 0.0448(3) 0.0178(11) Uani 1 1 d . . . . .
C8 C 0.2085(6) 0.7544(3) -0.0154(3) 0.0183(11) Uani 1 1 d . . . . .
C9 C -0.0061(6) 0.6128(3) -0.0709(3) 0.0162(10) Uani 1 1 d . . . . .
C10 C -0.0104(6) 0.9444(3) 0.1390(3) 0.0163(10) Uani 1 1 d . . . . .
H10 H 0.0714 0.9652 0.1774 0.020 Uiso 1 1 calc R . . . .
C11 C -0.1157(6) 1.0038(3) 0.0984(3) 0.0201(11) Uani 1 1 d . . . . .
H11 H -0.1046 1.0634 0.1089 0.024 Uiso 1 1 calc R . . . .
C12 C -0.2383(6) 0.9726(4) 0.0419(3) 0.0221(12) Uani 1 1 d . . . . .
H12 H -0.3114 1.0110 0.0139 0.027 Uiso 1 1 calc R . . . .
C13 C -0.2503(6) 0.8840(3) 0.0276(3) 0.0174(10) Uani 1 1 d . . . . .
H13 H -0.3316 0.8621 -0.0104 0.021 Uiso 1 1 calc R . . . .
C14 C -0.1399(5) 0.8270(3) 0.0703(3) 0.0131(10) Uani 1 1 d . . . . .
C15 C -0.1390(5) 0.7322(3) 0.0556(3) 0.0125(10) Uani 1 1 d . . . . .
C16 C -0.2888(6) 0.6879(4) 0.0517(3) 0.0156(10) Uani 1 1 d . . . . .
H16A H -0.310(6) 0.632(4) 0.017(4) 0.031(16) Uiso 1 1 d . . . . .
H16B H -0.396(6) 0.714(4) 0.065(3) 0.029(15) Uiso 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 Os2 2.8576(3) . ?
Os1 Os3 2.7913(3) . ?
Os1 N1 2.162(4) . ?
Os1 C1 1.919(5) . ?
Os1 C2 1.897(5) . ?
Os1 C3 1.874(5) . ?
Os2 Os3 2.8581(2) . ?
Os2 C4 1.936(5) . ?
Os2 C5 1.904(5) . ?
Os2 C6 1.910(5) . ?
Os2 C15 2.242(4) . ?
Os2 C16 2.306(5) . ?
Os3 C7 1.928(5) . ?
Os3 C8 1.877(5) . ?
Os3 C9 1.924(5) . ?
Os3 C15 2.122(4) . ?
O1 C1 1.138(6) . ?
O2 C2 1.147(6) . ?
O3 C3 1.156(6) . ?
O4 C4 1.126(6) . ?
O5 C5 1.140(6) . ?
O6 C6 1.145(6) . ?
O7 C7 1.134(6) . ?
O8 C8 1.152(6) . ?
O9 C9 1.133(6) . ?
N1 C10 1.331(6) . ?
N1 C14 1.348(6) . ?
C10 C11 1.383(7) . ?
C11 C12 1.385(7) . ?
C12 C13 1.375(7) . ?
C13 C14 1.399(6) . ?
C14 C15 1.466(6) . ?
C15 C16 1.393(7) . ?

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
Os3 Os1 Os2 60.777(6) . . ?
N1 Os1 Os2 86.03(10) . . ?
N1 Os1 Os3 85.64(10) . . ?
C1 Os1 Os2 93.90(14) . . ?
C1 Os1 Os3 154.65(14) . . ?
C1 Os1 N1 91.91(17) . . ?
C2 Os1 Os2 164.39(16) . . ?
C2 Os1 Os3 104.19(15) . . ?
C2 Os1 N1 88.74(18) . . ?
C2 Os1 C1 101.0(2) . . ?
C3 Os1 Os2 93.41(14) . . ?
C3 Os1 Os3 88.15(15) . . ?
C3 Os1 N1 173.17(18) . . ?
C3 Os1 C1 94.9(2) . . ?
C3 Os1 C2 90.0(2) . . ?
Os1 Os2 Os3 58.466(6) . . ?
C4 Os2 Os1 164.69(14) . . ?
C4 Os2 Os3 115.77(13) . . ?
C4 Os2 C15 116.53(19) . . ?
C4 Os2 C16 83.36(19) . . ?
C5 Os2 Os1 91.09(15) . . ?
C5 Os2 Os3 136.35(15) . . ?
C5 Os2 C4 100.8(2) . . ?
C5 Os2 C6 91.7(2) . . ?
C5 Os2 C15 96.05(19) . . ?
C5 Os2 C16 90.3(2) . . ?
C6 Os2 Os1 78.40(14) . . ?
C6 Os2 Os3 109.40(13) . . ?
C6 Os2 C4 91.5(2) . . ?
C6 Os2 C15 148.67(18) . . ?
C6 Os2 C16 174.75(19) . . ?
C15 Os2 Os1 71.17(12) . . ?
C15 Os2 Os3 47.29(11) . . ?
C15 Os2 C16 35.63(17) . . ?
C16 Os2 Os1 106.40(13) . . ?
C16 Os2 Os3 72.13(12) . . ?
Os1 Os3 Os2 60.758(6) . . ?
C7 Os3 Os1 99.04(15) . . ?
C7 Os3 Os2 112.99(14) . . ?
C7 Os3 C15 163.92(19) . . ?
C8 Os3 Os1 82.76(15) . . ?
C8 Os3 Os2 137.12(14) . . ?
C8 Os3 C7 93.1(2) . . ?
C8 Os3 C9 99.0(2) . . ?
C8 Os3 C15 100.27(19) . . ?
C9 Os3 Os1 165.28(14) . . ?
C9 Os3 Os2 110.92(13) . . ?
C9 Os3 C7 95.5(2) . . ?
C9 Os3 C15 91.19(19) . . ?
C15 Os3 Os1 74.14(13) . . ?
C15 Os3 Os2 50.93(12) . . ?
C10 N1 Os1 124.3(3) . . ?
C10 N1 C14 119.9(4) . . ?
C14 N1 Os1 115.8(3) . . ?
O1 C1 Os1 176.8(5) . . ?
O2 C2 Os1 179.4(5) . . ?
O3 C3 Os1 178.4(4) . . ?
O4 C4 Os2 175.1(4) . . ?
O5 C5 Os2 176.4(4) . . ?
O6 C6 Os2 176.8(4) . . ?
O7 C7 Os3 176.4(5) . . ?
O8 C8 Os3 178.6(4) . . ?
O9 C9 Os3 174.7(4) . . ?
N1 C10 C11 122.4(5) . . ?
C10 C11 C12 118.7(5) . . ?
C13 C12 C11 119.0(5) . . ?
C12 C13 C14 119.9(5) . . ?
N1 C14 C13 120.2(4) . . ?
N1 C14 C15 116.4(4) . . ?
C13 C14 C15 123.4(4) . . ?
Os3 C15 Os2 81.78(15) . . ?
C14 C15 Os2 116.7(3) . . ?
C14 C15 Os3 120.9(3) . . ?
C16 C15 Os2 74.7(3) . . ?
C16 C15 Os3 120.5(4) . . ?
C16 C15 C14 118.6(4) . . ?
C15 C16 Os2 69.7(3) . . ?


_olex2_date_sample_data_collection 2018-02-08
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id xstr0818
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.084
_oxdiff_exptl_absorpt_empirical_full_min 0.701
