# Electronic Supplementary Material (ESI) for RSC Chemical Biology.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_Os245
_database_code_depnum_ccdc_archive 'CCDC 2201801'
loop_
_audit_author_name
_audit_author_address
'Joshua J. Woods'
;Lawrence Berkeley National Laboratory
United States of America
;
_audit_update_record             
;
2022-08-16 deposited with the CCDC.	2022-11-07 downloaded from the CCDC.
;
_audit_creation_date             2021-06-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl2 H24 N9 Os2, 3(Cl), O'
_chemical_formula_sum            'Cl5 H24 N9 O Os2'
_chemical_formula_weight         723.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         Os2N9H24Cl5
_chemical_oxdiff_usercomment     
'Grown by vapor diffusion of Acetone into H2O w/ NaBPh4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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      orthorhombic
_space_group_IT_number           65
_space_group_name_H-M_alt        'C m m m'
_space_group_name_Hall           '-C 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'

_cell_length_a                   7.77840(10)
_cell_length_b                   16.3909(2)
_cell_length_c                   7.70290(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     982.08(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18296
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      31.6520
_cell_measurement_theta_min      2.9200
_shelx_estimated_absorpt_T_max   0.670
_shelx_estimated_absorpt_T_min   0.301
_exptl_absorpt_coefficient_mu    13.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    2.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             664
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 2 11 0.0210
11 0 -2 0.0495
0 -2 -11 0.0565
6 -1 -9 0.0583
-11 -1 -3 0.0590
-9 1 7 0.0480
8 1 7 0.0449
-9 -1 -7 0.0599
-1 -20 6 0.0082
-2 23 0 0.0233
2 -23 -1 0.0085
-7 -14 -5 0.0402

_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.032
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.6635 1.6728 10.8100 0.1095 -0.3697 0.9227
10.7411 0.0554 -2.1846 0.2442 -0.8234 -0.5122
-0.4296 -1.6661 -10.8217 -0.1039 0.3507 -0.9307
5.7409 -1.2003 -9.2310 0.0609 -0.2052 -0.9768
-10.5322 -0.8396 -3.0062 -0.2839 0.9574 0.0534
-8.6642 0.6998 6.6435 -0.1549 0.5220 0.8388
8.0688 1.4097 7.3283 0.2609 -0.8798 0.3973
-8.6866 -1.3215 -6.6036 -0.2697 0.9098 -0.3156
-0.5069 -19.6715 5.6752 -0.8225 -0.3409 0.4553
-1.8003 22.7853 0.3939 0.9134 0.3787 0.1490
1.9997 -22.6251 -1.0100 -0.9035 -0.3746 -0.2081
-6.9011 -14.1093 -5.2214 -0.7610 0.5836 -0.2834

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22952
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.604
_diffrn_reflns_theta_min         2.485
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#---------
  1  ω    -44.00  11.00   0.50    7.20    ---------    4.12   0.00   0.00  110
  2  ω    -24.00  67.00   0.50    7.20    ---------   -4.59  77.00  60.00  182
  3  ω     -9.00  67.00   0.50    7.20    ---------   -4.59  19.00 150.00  152
  4  ω    -23.00  26.00   0.50    7.20    ---------   -4.59 -99.00 120.00   98
  5  ω    -23.00  26.00   0.50    7.20    ---------   -4.59 -99.00 150.00   98
  6  ω    -53.00   2.00   0.50    7.20    ---------   -4.59   0.00  60.00  110
  7  ω    -53.00   2.00   0.50    7.20    ---------   -4.59   0.00 -30.00  110
  8  ω     -9.00  67.00   0.50    7.20    -   -4.59  19.00 -90.00  152
  9  ω    -10.00  68.00   0.50    7.20    -   -4.59  20.00-155.75  156
 10  ω     -9.00  67.00   0.50    7.20    -   -4.59  19.00-180.00  152
 11  ω    -23.00  26.00   0.50    7.20    -   -4.59 -99.00-120.00   98
 12  ω    -23.00  26.00   0.50    7.20    -   -4.59 -99.00-180.00   98
 13  ω    -23.00  26.00   0.50    7.20    -   -4.59 -99.00 -30.00   98
 14  ω    -53.00   2.00   0.50    7.20    -   -4.59   0.00  90.00  110
 15  ω    -66.00  24.00   0.50    7.20    -    4.12 -77.00  60.00  180
 16  ω    -66.00  24.00   0.50    7.20    -    4.12 -77.00 -90.00  180
 17  ω    -67.00   5.00   0.50    7.20    -    4.12 -19.00-180.00  144
 18  ω    -66.00  10.00   0.50    7.20    -    4.12 -37.00 -60.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0229779000
_diffrn_orient_matrix_UB_12      0.0418659000
_diffrn_orient_matrix_UB_13      0.0022440000
_diffrn_orient_matrix_UB_21      -0.0829671000
_diffrn_orient_matrix_UB_22      0.0105967000
_diffrn_orient_matrix_UB_23      -0.0307492000
_diffrn_orient_matrix_UB_31      -0.0300506000
_diffrn_orient_matrix_UB_32      0.0026657000
_diffrn_orient_matrix_UB_33      0.0867843000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                866
_reflns_number_total             912
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.620
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.308
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.267
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         912
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0264
_refine_ls_restrained_S_all      1.267
_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)+(0.0367P)²+8.2193P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0710
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2. Others
 Fixed Sof: Cl4(0.125) O1(0.125)
3.a Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Os Os 0.500000 0.39209(2) 1.000000 0.01209(11) Uani 1 4 d S T P . .
Cl1 Cl 0.500000 0.24335(12) 1.000000 0.0230(4) Uani 1 4 d S T P . .
Cl2 Cl 1.000000 0.500000 1.000000 0.0420(11) Uani 1 8 d S T P . .
Cl3 Cl 0.500000 0.500000 0.500000 0.0447(11) Uani 1 8 d S T P . .
Cl4 Cl 0.6819(17) 0.2440(7) 0.500000 0.061(4) Uani 0.25 2 d S T P . .
O1 O 0.000000 0.619(3) 0.500000 0.15(3) Uani 0.5 4 d S T P . .
N1 N 0.500000 0.500000 1.000000 0.0131(17) Uani 1 8 d S T P . .
N2 N 0.3055(6) 0.3855(2) 0.8071(6) 0.0252(9) Uani 1 1 d . . . . .
H2A H 0.343960 0.409247 0.707632 0.030 Uiso 1 1 calc R U . . .
H2B H 0.209949 0.412162 0.844986 0.030 Uiso 1 1 calc R U . . .
H2C H 0.279205 0.332331 0.786078 0.030 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os Cl1 2.438(2) . ?
Os N1 1.7688(3) . ?
Os N2 2.123(4) 3_657 ?
Os N2 2.123(4) . ?
Os N2 2.123(4) 10_557 ?
Os N2 2.123(4) 12_655 ?
Cl4 Cl4 1.08(3) 13_656 ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?

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 Os Cl1 180.0 . . ?
N1 Os N2 92.91(10) . 10_557 ?
N1 Os N2 92.91(10) . 3_657 ?
N1 Os N2 92.91(10) . . ?
N1 Os N2 92.91(10) . 12_655 ?
N2 Os Cl1 87.09(10) 12_655 . ?
N2 Os Cl1 87.09(10) . . ?
N2 Os Cl1 87.09(10) 10_557 . ?
N2 Os Cl1 87.09(10) 3_657 . ?
N2 Os N2 90.9(3) . 12_655 ?
N2 Os N2 88.8(3) 3_657 12_655 ?
N2 Os N2 90.9(3) 3_657 10_557 ?
N2 Os N2 174.2(2) 12_655 10_557 ?
N2 Os N2 174.2(2) . 3_657 ?
N2 Os N2 88.8(3) . 10_557 ?
Os N1 Os 180.0 9_667 . ?
Os N2 H2A 109.5 . . ?
Os N2 H2B 109.5 . . ?
Os N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?

_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 2.256
_oxdiff_exptl_absorpt_empirical_full_min 0.725
####################################################################### 
# 
# 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_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 2201803'
loop_
_audit_author_name
_audit_author_address
'Joshua J. Woods'
;Lawrence Berkeley National Laboratory
United States of America
;
_audit_update_record             
;
2022-08-16 deposited with the CCDC.	2022-11-07 downloaded from the CCDC.
;
_audit_creation_date             2017-07-11
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl H26 N10 Os2, 3(C H3 O3 S), 0.5(H2 O2), Cl'
_chemical_formula_sum            'C3 H36 Cl2 N10 O10 Os2 S3'
_chemical_formula_weight         919.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         C3H24Cl2N9O11Os2S3F9
_chemical_oxdiff_usercomment     
'Crystallized from THF diffusion into methanesulfonic acid'
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'
S S 0.1246 0.1234 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   18.1826(5)
_cell_length_b                   7.8130(2)
_cell_length_c                   17.3198(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2460.46(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5345
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.7470
_cell_measurement_theta_min      2.2350
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.848
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    2.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1752
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
18 4 14 0.0269
18 0 -18 0.0093
-17 -4 -15 0.0343
19 0 17 0.0112
-19 0 -17 0.0112
0 11 0 0.0452
-2 -11 -2 0.0704
-18 0 18 0.0065
10 -1 22 0.0067

_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.016
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
18.4306 4.1825 14.1941 -0.0751 -0.0215 0.9969
17.5578 0.0163 -17.8018 -0.9588 -0.2839 -0.0093
-17.2635 -4.1913 -15.4556 0.0091 0.0019 -1.0000
19.0000 -0.0000 17.0000 -0.1182 0.3694 0.9405
-19.0000 0.0000 -17.0000 0.1182 -0.3694 -0.9405
0.0000 11.0000 0.0000 0.2573 -0.8864 0.3809
-2.0000 -11.0000 -2.0000 -0.2502 0.8436 -0.4854
-18.0000 0.0000 18.0000 0.9770 0.2851 0.0036
10.0000 -1.0000 22.0000 0.2454 0.5180 0.8028

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11897
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.248
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         2.240
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     10.00  68.00   0.50   23.50    --    3.71  64.00  63.00  116
  2  ω    -19.00  15.00   0.50   23.50    --   -4.80  93.00 162.00   68
  3  ω    -22.00   5.00   0.50   23.50    --   -4.80 -99.00 -60.00   54
  4  ω    -26.00  23.00   0.50   23.50    --   -4.80 -99.00-120.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0289154000
_diffrn_orient_matrix_UB_12      0.0233949000
_diffrn_orient_matrix_UB_13      0.0253622000
_diffrn_orient_matrix_UB_21      0.0027822000
_diffrn_orient_matrix_UB_22      -0.0805780000
_diffrn_orient_matrix_UB_23      0.0186191000
_diffrn_orient_matrix_UB_31      0.0260327000
_diffrn_orient_matrix_UB_32      0.0346265000
_diffrn_orient_matrix_UB_33      0.0262307000
_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              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2185
_reflns_number_total             2403
_reflns_odcompleteness_completeness 99.79
_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 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.457
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2403
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²+4.3384P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0516
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-H7
 0.84 with sigma of 0.02
3. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5) H3A(0.5) H3E(0.5) H3F(0.5) H2E(0.5)
 H2F(0.5) H1A(0.5) H1B(0.5) H1C(0.5) H7(0.5)
4.a Me refined with riding coordinates:
 C3(H3D,H3E,H3F), C2(H2D,H2E,H2F)
4.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C), N5(H5A,H5B,H5C), N6(H6A,
 H6B,H6C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.89269(2) 0.250000 0.42725(2) 0.01123(8) Uani 1 2 d S T P . .
Os2 Os 0.72827(2) 0.250000 0.31789(2) 0.01071(8) Uani 1 2 d S T P . .
Cl1 Cl 1.01008(7) 0.250000 0.49501(10) 0.0194(3) Uani 1 2 d S T P . .
N1 N 0.8093(2) 0.250000 0.3758(3) 0.0129(10) Uani 1 2 d S T P . .
N2 N 0.6313(3) 0.250000 0.2419(3) 0.0163(11) Uani 1 2 d S T P . .
H2A H 0.592677 0.200573 0.266825 0.020 Uiso 0.5 1 calc GR . . A -1
H2B H 0.641488 0.189792 0.198181 0.020 Uiso 0.5 1 calc GR . . A -1
H2C H 0.619483 0.359635 0.229128 0.020 Uiso 0.5 1 calc GR . . A -1
N3 N 0.67512(17) 0.0540(4) 0.3830(2) 0.0151(7) Uani 1 1 d . . . . .
H3A H 0.686623 -0.050100 0.362755 0.018 Uiso 0.5 1 calc GR . . . .
H3B H 0.625553 0.069564 0.381114 0.018 Uiso 1 1 calc GR . . . .
H3C H 0.690503 0.058840 0.432967 0.018 Uiso 1 1 calc GR . . . .
N4 N 0.76990(17) 0.4460(5) 0.2455(2) 0.0178(8) Uani 1 1 d . . . . .
H4A H 0.735464 0.474044 0.209538 0.021 Uiso 1 1 calc GR . . . .
H4B H 0.811320 0.408324 0.221403 0.021 Uiso 1 1 calc GR . . . .
H4C H 0.780788 0.539781 0.274484 0.021 Uiso 1 1 calc GR . . . .
N5 N 0.85827(17) 0.0602(4) 0.5063(2) 0.0160(7) Uani 1 1 d . . . . .
H5A H 0.863819 -0.045072 0.484564 0.019 Uiso 1 1 calc GR . . . .
H5B H 0.810122 0.077043 0.518463 0.019 Uiso 1 1 calc GR . . . .
H5C H 0.886037 0.066825 0.549906 0.019 Uiso 1 1 calc GR . . . .
N6 N 0.93766(17) 0.4436(4) 0.3552(2) 0.0161(7) Uani 1 1 d . . . . .
H6A H 0.938349 0.406290 0.305425 0.019 Uiso 1 1 calc GR . . . .
H6B H 0.984329 0.467839 0.370699 0.019 Uiso 1 1 calc GR . . . .
H6C H 0.909547 0.539711 0.358574 0.019 Uiso 1 1 calc GR . . . .
S3 S 0.33152(8) 0.750000 0.41293(10) 0.0194(3) Uani 1 2 d S T P . .
O5 O 0.3360(3) 0.750000 0.3290(3) 0.0279(11) Uani 1 2 d S T P . .
O6 O 0.29687(15) 0.5950(4) 0.4440(2) 0.0253(7) Uani 1 1 d . . . . .
C3 C 0.4221(3) 0.750000 0.4482(4) 0.0251(15) Uani 1 2 d S T P . .
H3D H 0.421350 0.750000 0.504740 0.038 Uiso 0.5 1 calc RS T P B -1
H3E H 0.447818 0.647585 0.429700 0.038 Uiso 0.5 1 calc R . . B -1
H3F H 0.447818 0.852415 0.429700 0.038 Uiso 0.5 1 calc R . . B -1
S2 S 0.40150(8) 0.250000 0.78172(10) 0.0187(3) Uani 1 2 d S T P . .
O3 O 0.39704(17) 0.4059(5) 0.8279(2) 0.0290(8) Uani 1 1 d . . . . .
O4 O 0.3491(2) 0.250000 0.7183(3) 0.0269(11) Uani 1 2 d S T P . .
C2 C 0.4899(3) 0.250000 0.7391(4) 0.0267(16) Uani 1 2 d S T P . .
H2D H 0.527387 0.250000 0.779770 0.040 Uiso 0.5 1 calc RS T P C -1
H2E H 0.495599 0.147585 0.707040 0.040 Uiso 0.5 1 calc R . . C -1
H2F H 0.495599 0.352415 0.707040 0.040 Uiso 0.5 1 calc R . . C -1
S1 S 0.46583(8) 0.250000 0.36428(10) 0.0179(3) Uani 1 2 d S T P . .
O1 O 0.51062(15) 0.4044(4) 0.3675(2) 0.0276(8) Uani 1 1 d . . . . .
O2 O 0.4159(2) 0.250000 0.2985(3) 0.0240(10) Uani 1 2 d S T P . .
C1 C 0.4096(4) 0.250000 0.4475(5) 0.0298(16) Uani 1 2 d S T P . .
H1A H 0.373461 0.342622 0.443726 0.045 Uiso 0.5 1 calc GR . . D -1
H1B H 0.440242 0.267365 0.493424 0.045 Uiso 0.5 1 calc GR . . D -1
H1C H 0.384004 0.140013 0.451572 0.045 Uiso 0.5 1 calc GR . . D -1
O7 O 0.2294(3) 0.250000 0.4030(5) 0.0553(17) Uani 1 2 d DS T P . .
H7 H 0.256(6) 0.185(14) 0.432(7) 0.066 Uiso 0.5 1 d DR . . E -1
Cl2 Cl 0.81349(7) 0.750000 0.38140(10) 0.0213(3) Uani 1 2 d S T 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 Cl1 2.4357(13) . ?
Os1 N1 1.759(5) . ?
Os1 N5 2.113(3) . ?
Os1 N5 2.113(3) 7_565 ?
Os1 N6 2.125(3) 7_565 ?
Os1 N6 2.125(3) . ?
Os2 N1 1.782(5) . ?
Os2 N2 2.201(5) . ?
Os2 N3 2.134(3) 7_565 ?
Os2 N3 2.134(3) . ?
Os2 N4 2.119(4) 7_565 ?
Os2 N4 2.119(4) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 H4C 0.9100 . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 H5C 0.9100 . ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
N6 H6C 0.9100 . ?
S3 O5 1.456(5) . ?
S3 O6 1.467(3) . ?
S3 O6 1.467(3) 7_575 ?
S3 C3 1.757(6) . ?
C3 H3D 0.9800 . ?
C3 H3E 0.9800 . ?
C3 H3F 0.9800 . ?
S2 O3 1.460(4) . ?
S2 O3 1.460(4) 7_565 ?
S2 O4 1.453(5) . ?
S2 C2 1.768(6) . ?
C2 H2D 0.9800 . ?
C2 H2E 0.9800 . ?
C2 H2F 0.9800 . ?
S1 O1 1.457(3) . ?
S1 O1 1.457(3) 7_565 ?
S1 O2 1.458(5) . ?
S1 C1 1.767(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
O7 H7 0.86(2) . ?

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 Cl1 178.39(16) . . ?
N1 Os1 N5 94.16(15) . . ?
N1 Os1 N5 94.16(15) . 7_565 ?
N1 Os1 N6 91.98(14) . . ?
N1 Os1 N6 91.97(14) . 7_565 ?
N5 Os1 Cl1 86.99(9) 7_565 . ?
N5 Os1 Cl1 86.98(9) . . ?
N5 Os1 N5 89.1(2) . 7_565 ?
N5 Os1 N6 89.71(14) 7_565 . ?
N5 Os1 N6 89.70(14) . 7_565 ?
N5 Os1 N6 173.82(13) . . ?
N5 Os1 N6 173.83(13) 7_565 7_565 ?
N6 Os1 Cl1 86.90(9) 7_565 . ?
N6 Os1 Cl1 86.90(9) . . ?
N6 Os1 N6 90.79(19) . 7_565 ?
N1 Os2 N2 177.5(2) . . ?
N1 Os2 N3 94.39(14) . . ?
N1 Os2 N3 94.39(14) . 7_565 ?
N1 Os2 N4 92.18(14) . 7_565 ?
N1 Os2 N4 92.18(14) . . ?
N3 Os2 N2 87.32(13) 7_565 . ?
N3 Os2 N2 87.32(13) . . ?
N3 Os2 N3 91.75(19) . 7_565 ?
N4 Os2 N2 86.12(13) . . ?
N4 Os2 N2 86.12(13) 7_565 . ?
N4 Os2 N3 87.47(14) 7_565 . ?
N4 Os2 N3 173.42(13) . . ?
N4 Os2 N3 87.47(14) . 7_565 ?
N4 Os2 N3 173.42(13) 7_565 7_565 ?
N4 Os2 N4 92.6(2) . 7_565 ?
Os1 N1 Os2 176.1(3) . . ?
Os2 N2 H2A 109.5 . . ?
Os2 N2 H2B 109.5 . . ?
Os2 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
Os2 N3 H3A 109.5 . . ?
Os2 N3 H3B 109.5 . . ?
Os2 N3 H3C 109.5 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Os2 N4 H4A 109.5 . . ?
Os2 N4 H4B 109.5 . . ?
Os2 N4 H4C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
Os1 N5 H5A 109.5 . . ?
Os1 N5 H5B 109.5 . . ?
Os1 N5 H5C 109.5 . . ?
H5A N5 H5B 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
Os1 N6 H6A 109.5 . . ?
Os1 N6 H6B 109.5 . . ?
Os1 N6 H6C 109.5 . . ?
H6A N6 H6B 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
O5 S3 O6 112.97(17) . . ?
O5 S3 O6 112.97(17) . 7_575 ?
O5 S3 C3 107.1(3) . . ?
O6 S3 O6 111.2(3) . 7_575 ?
O6 S3 C3 105.98(19) . . ?
O6 S3 C3 105.98(19) 7_575 . ?
S3 C3 H3D 109.5 . . ?
S3 C3 H3E 109.5 . . ?
S3 C3 H3F 109.5 . . ?
H3D C3 H3E 109.5 . . ?
H3D C3 H3F 109.5 . . ?
H3E C3 H3F 109.5 . . ?
O3 S2 O3 113.1(3) . 7_565 ?
O3 S2 C2 106.20(19) . . ?
O3 S2 C2 106.20(19) 7_565 . ?
O4 S2 O3 112.18(17) . . ?
O4 S2 O3 112.18(17) . 7_565 ?
O4 S2 C2 106.3(3) . . ?
S2 C2 H2D 109.5 . . ?
S2 C2 H2E 109.5 . . ?
S2 C2 H2F 109.5 . . ?
H2D C2 H2E 109.5 . . ?
H2D C2 H2F 109.5 . . ?
H2E C2 H2F 109.5 . . ?
O1 S1 O1 111.8(2) . 7_565 ?
O1 S1 O2 112.24(17) . . ?
O1 S1 O2 112.24(17) 7_565 . ?
O1 S1 C1 107.0(2) . . ?
O1 S1 C1 107.0(2) 7_565 . ?
O2 S1 C1 106.1(3) . . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
S1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

_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 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.901
####################################################################### 
# 
# 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_Os245_prime
_database_code_depnum_ccdc_archive 'CCDC 2201802'
loop_
_audit_author_name
_audit_author_address
'Joshua J. Woods'
;Lawrence Berkeley National Laboratory
United States of America
;
_audit_update_record             
;
2022-08-16 deposited with the CCDC.	2022-11-07 downloaded from the CCDC.
;
_audit_creation_date             2021-08-31
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(H14 N4.5 O Os), 5(N O3), H2 O'
_chemical_formula_sum            'H30 N14 O18 Os2'
_chemical_formula_weight         894.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'H120  N56  O72  Os8  '
_chemical_oxdiff_usercomment     
'Grown by vapor diffusion of acetone into water'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   15.3326(2)
_cell_length_b                   10.76340(10)
_cell_length_c                   14.9970(2)
_cell_angle_alpha                90
_cell_angle_beta                 111.5530(10)
_cell_angle_gamma                90
_cell_volume                     2301.91(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    76026
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      31.5510
_cell_measurement_theta_min      2.8540
_shelx_estimated_absorpt_T_max   0.510
_shelx_estimated_absorpt_T_min   0.269
_exptl_absorpt_coefficient_mu    11.135
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    2.582
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
16 8 2 0.0438
-16 10 8 0.0406
-18 0 17 0.0369
-8 -10 16 0.0437
6 11 -15 0.0483
19 -3 -16 0.0615
-8 13 9 0.0330
-10 1 -13 0.0628
9 1 15 0.0766
0 10 15 0.0559
-13 8 -8 0.0685
-8 13 8 0.0330
1 -2 -1 0.0289

_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.065
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
15.6098 8.4984 2.3777 0.9996 -0.0259 0.0109
-16.4718 9.6515 8.3022 -0.1645 -0.3456 0.9238
-18.0448 0.2589 17.3054 -0.3959 -0.8308 0.3913
-7.8318 -10.1037 15.6430 -0.3854 -0.8084 -0.4450
6.0637 10.9620 -14.6105 0.3640 0.7635 0.5335
18.6657 -2.6340 -16.0173 0.3600 0.7556 -0.5472
-7.6700 13.4116 8.7672 0.3444 -0.3267 0.8801
-10.3889 1.1759 -13.4382 -0.6479 0.6144 0.4503
9.0421 0.9053 14.5697 0.6904 -0.6547 -0.3077
0.2693 9.7713 14.9520 0.6597 -0.6257 0.4163
-12.9462 7.5552 -7.6728 -0.4080 0.3868 0.8270
-8.1753 13.4708 8.1165 0.3130 -0.2970 0.9021
1.0000 -2.0000 -1.0000 -0.0513 0.0342 -0.1295

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            104889
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.363
_diffrn_reflns_theta_min         2.390
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  27.00   0.50    1.76    --    5.48 -76.00 -61.00  188
  2  ω    -27.00  66.00   0.50    1.76    --   -5.95  76.00  65.00  186
  3  ω    -78.00  15.00   0.50    1.76    --   -5.95 -76.00 -61.00  186
  4  ω    -23.00  38.00   0.50    1.76    --    5.48 -99.00-120.00  122
  5  ω    -16.00  78.00   0.50    1.76    --    5.48  76.00  65.00  188
  6  ω    -23.00  26.00   0.50    1.76    --   -5.95 -99.00 150.00   98
  7  ω    -17.00  68.00   0.50    1.76    --   -5.95  29.00  78.69  170
  8  ω    -17.00  68.00   0.50    1.76    --   -5.95  29.00-110.57  170
  9  ω    -17.00  67.00   0.50    1.76    --   -5.95  30.00  34.70  168
 10  ω    -16.00  68.00   0.50    1.76    --   -5.95  26.00-171.70  168
 11  ω    -23.00  26.00   0.50    1.76    --   -5.95 -99.00  90.00   98
 12  ω    -16.00  69.00   0.50    1.76    --   -5.95  19.00 150.00  170
 13  ω    -17.00  68.00   0.50    1.76    --   -5.95  28.00  -6.76  170
 14  ω    -23.00  26.00   0.50    1.76    --   -5.95 -99.00 -30.00   98
 15  ω    -16.00  67.00   0.50    1.76    --   -5.95  33.00 -61.70  166
 16  ω    -67.00 -15.00   0.50    1.76    --    5.48 -37.00 120.00  104
 17  ω      6.00  47.00   0.50    1.76    --    5.48-115.00  43.53   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0412074000
_diffrn_orient_matrix_UB_12      0.0364644000
_diffrn_orient_matrix_UB_13      0.0195474000
_diffrn_orient_matrix_UB_21      0.0016488000
_diffrn_orient_matrix_UB_22      0.0069063000
_diffrn_orient_matrix_UB_23      -0.0463903000
_diffrn_orient_matrix_UB_31      -0.0278339000
_diffrn_orient_matrix_UB_32      0.0544312000
_diffrn_orient_matrix_UB_33      -0.0072256000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6429
_reflns_number_total             6911
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.854
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6911
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0207
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0146P)²+6.9063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0418
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O2-H2E = O2-H2D = O1-H1B = O1-H1A = O3-H3E = O3-H3D
 0.84 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C), N5(H5A,H5B,H5C), N7(H7A,
 H7B,H7C), N8(H8A,H8B,H8C), N9(H9A,H9B,H9C), N10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.02709(2) 0.34015(2) 0.51052(2) 0.00770(3) Uani 1 1 d . . . . .
O1 O 0.05859(14) 0.14633(17) 0.52629(15) 0.0127(4) Uani 1 1 d D . . . .
H1A H 0.073(2) 0.106(3) 0.5777(18) 0.015 Uiso 1 1 d D U . . .
H1B H 0.077(2) 0.109(3) 0.487(2) 0.015 Uiso 1 1 d D U . . .
O4 O 0.19028(17) -0.0375(2) 0.33269(17) 0.0260(5) Uani 1 1 d . . . . .
O5 O 0.11478(19) -0.0215(2) 0.42952(19) 0.0302(6) Uani 1 1 d . . . . .
O6 O 0.14750(18) 0.1431(2) 0.36629(16) 0.0246(5) Uani 1 1 d . . . . .
O13 O 0.27904(17) 0.1938(2) 0.69432(17) 0.0261(5) Uani 1 1 d . . . . .
O14 O 0.29953(17) 0.1491(2) 0.56263(17) 0.0268(5) Uani 1 1 d . . . . .
O15 O 0.42010(15) 0.1849(2) 0.69223(16) 0.0224(4) Uani 1 1 d . . . . .
N1 N 0.000000 0.500000 0.500000 0.0102(6) Uani 1 2 d S . P . .
N2 N -0.04446(16) 0.2971(2) 0.36286(16) 0.0127(4) Uani 1 1 d . . . . .
H2A H -0.055308 0.213827 0.356103 0.015 Uiso 1 1 calc R U . . .
H2B H -0.008593 0.320443 0.329037 0.015 Uiso 1 1 calc R U . . .
H2C H -0.100059 0.338501 0.340357 0.015 Uiso 1 1 calc R U . . .
N3 N -0.09461(16) 0.2908(2) 0.53879(17) 0.0130(4) Uani 1 1 d . . . . .
H3A H -0.094011 0.330851 0.592450 0.016 Uiso 1 1 calc R U . . .
H3B H -0.095131 0.207251 0.547891 0.016 Uiso 1 1 calc R U . . .
H3C H -0.146746 0.313174 0.488127 0.016 Uiso 1 1 calc R U . . .
N4 N 0.10474(17) 0.3545(2) 0.65886(17) 0.0134(4) Uani 1 1 d . . . . .
H4A H 0.069935 0.394671 0.687662 0.016 Uiso 1 1 calc R U . . .
H4B H 0.158395 0.397877 0.668564 0.016 Uiso 1 1 calc R U . . .
H4C H 0.119428 0.277061 0.684372 0.016 Uiso 1 1 calc R U . . .
N5 N 0.15349(16) 0.3641(2) 0.48587(17) 0.0130(4) Uani 1 1 d . . . . .
H5A H 0.191435 0.418008 0.529879 0.016 Uiso 1 1 calc R U . . .
H5B H 0.140388 0.395143 0.425895 0.016 Uiso 1 1 calc R U . . .
H5C H 0.182961 0.289565 0.491260 0.016 Uiso 1 1 calc R U . . .
N11 N 0.15092(17) 0.0282(2) 0.37564(17) 0.0159(5) Uani 1 1 d . . . . .
N14 N 0.33073(17) 0.1764(2) 0.64932(18) 0.0159(5) Uani 1 1 d . . . . .
Os2 Os 0.50860(2) 0.14234(2) 0.44506(2) 0.01189(3) Uani 1 1 d . . . . .
O2 O 0.52129(16) 0.3135(2) 0.37903(17) 0.0218(4) Uani 1 1 d D . . . .
H2D H 0.487(2) 0.331(4) 0.3239(17) 0.026 Uiso 1 1 d D U . . .
H2E H 0.541(3) 0.382(2) 0.407(3) 0.026 Uiso 1 1 d D U . . .
N6 N 0.500000 0.000000 0.500000 0.0127(6) Uani 1 2 d S . P . .
N7 N 0.49962(18) 0.0677(2) 0.31139(19) 0.0196(5) Uani 1 1 d . . . . .
H7A H 0.459202 0.114128 0.263117 0.024 Uiso 1 1 calc R U . . .
H7B H 0.478447 -0.011949 0.306344 0.024 Uiso 1 1 calc R U . . .
H7C H 0.557349 0.068848 0.307225 0.024 Uiso 1 1 calc R U . . .
N8 N 0.65740(18) 0.1384(3) 0.4895(2) 0.0253(6) Uani 1 1 d . . . . .
H8A H 0.682951 0.116989 0.552572 0.030 Uiso 1 1 calc R U . . .
H8B H 0.678516 0.214861 0.481144 0.030 Uiso 1 1 calc R U . . .
H8C H 0.674323 0.081627 0.453901 0.030 Uiso 1 1 calc R U . . .
N9 N 0.51632(19) 0.2549(2) 0.56327(18) 0.0194(5) Uani 1 1 d . . . . .
H9A H 0.491887 0.331154 0.541968 0.023 Uiso 1 1 calc R U . . .
H9B H 0.577293 0.263163 0.603059 0.023 Uiso 1 1 calc R U . . .
H9C H 0.483099 0.218831 0.595675 0.023 Uiso 1 1 calc R U . . .
N10 N 0.36117(17) 0.1685(2) 0.38861(18) 0.0167(5) Uani 1 1 d . . . . .
H10A H 0.333600 0.105504 0.347393 0.020 Uiso 1 1 calc R U . . .
H10B H 0.347372 0.242227 0.356817 0.020 Uiso 1 1 calc R U . . .
H10C H 0.339289 0.168902 0.437387 0.020 Uiso 1 1 calc R U . . .
O3 O 0.6721(3) 0.4116(3) 0.7697(4) 0.0646(12) Uani 1 1 d D . . . .
H3D H 0.706(4) 0.387(7) 0.827(2) 0.078 Uiso 1 1 d D U . . .
H3E H 0.717(3) 0.456(5) 0.768(5) 0.078 Uiso 1 1 d D U . . .
O7 O 0.89345(16) 0.4764(2) 0.82690(15) 0.0212(4) Uani 1 1 d . . . . .
O8 O 0.94422(18) 0.4421(2) 0.71176(18) 0.0305(6) Uani 1 1 d . . . . .
O9 O 0.9304(2) 0.6291(2) 0.7545(2) 0.0346(6) Uani 1 1 d . . . . .
N12 N 0.92206(18) 0.5159(2) 0.76387(17) 0.0164(5) Uani 1 1 d . . . . .
O10 O 0.2418(2) 0.6755(3) 0.6531(2) 0.0485(8) Uani 1 1 d . . . . .
O11 O 0.2893(2) 0.4817(3) 0.6748(2) 0.0407(7) Uani 1 1 d . . . . .
O12 O 0.35658(18) 0.6226(3) 0.7798(2) 0.0379(7) Uani 1 1 d . . . . .
N13 N 0.29608(19) 0.5921(3) 0.7017(2) 0.0264(6) Uani 1 1 d . . . . .
O16 O 0.40941(18) 0.4926(2) 0.5123(2) 0.0384(7) Uani 1 1 d . . . . .
O17 O 0.29079(19) 0.4274(2) 0.3895(2) 0.0349(6) Uani 1 1 d . . . . .
O18 O 0.2843(2) 0.6038(3) 0.4546(2) 0.0471(8) Uani 1 1 d . . . . .
N15 N 0.32731(19) 0.5077(2) 0.4511(2) 0.0245(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
Os1 O1 2.1348(18) . ?
Os1 N1 1.76340(9) . ?
Os1 N2 2.130(2) . ?
Os1 N3 2.127(2) . ?
Os1 N4 2.108(2) . ?
Os1 N5 2.118(2) . ?
O1 H1A 0.839(18) . ?
O1 H1B 0.845(18) . ?
O4 N11 1.251(3) . ?
O5 N11 1.255(3) . ?
O6 N11 1.243(3) . ?
O13 N14 1.229(3) . ?
O14 N14 1.244(3) . ?
O15 N14 1.285(3) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 H4C 0.9100 . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 H5C 0.9100 . ?
Os2 O2 2.134(2) . ?
Os2 N6 1.76729(10) . ?
Os2 N7 2.117(3) . ?
Os2 N8 2.129(3) . ?
Os2 N9 2.114(3) . ?
Os2 N10 2.121(2) . ?
O2 H2D 0.825(19) . ?
O2 H2E 0.840(19) . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?
N7 H7C 0.9100 . ?
N8 H8A 0.9100 . ?
N8 H8B 0.9100 . ?
N8 H8C 0.9100 . ?
N9 H9A 0.9100 . ?
N9 H9B 0.9100 . ?
N9 H9C 0.9100 . ?
N10 H10A 0.9100 . ?
N10 H10B 0.9100 . ?
N10 H10C 0.9100 . ?
O3 H3D 0.87(2) . ?
O3 H3E 0.84(2) . ?
O7 N12 1.254(3) . ?
O8 N12 1.246(3) . ?
O9 N12 1.238(3) . ?
O10 N13 1.258(4) . ?
O11 N13 1.247(4) . ?
O12 N13 1.242(4) . ?
O16 N15 1.267(4) . ?
O17 N15 1.239(4) . ?
O18 N15 1.238(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Os1 O1 178.50(5) . . ?
N1 Os1 N2 96.03(6) . . ?
N1 Os1 N3 93.81(6) . . ?
N1 Os1 N4 92.65(6) . . ?
N1 Os1 N5 93.78(6) . . ?
N2 Os1 O1 84.92(8) . . ?
N3 Os1 O1 85.03(8) . . ?
N3 Os1 N2 89.91(9) . . ?
N4 Os1 O1 86.42(8) . . ?
N4 Os1 N2 171.29(9) . . ?
N4 Os1 N3 90.27(9) . . ?
N4 Os1 N5 88.68(9) . . ?
N5 Os1 O1 87.37(8) . . ?
N5 Os1 N2 90.00(9) . . ?
N5 Os1 N3 172.37(9) . . ?
Os1 O1 H1A 125(3) . . ?
Os1 O1 H1B 121(3) . . ?
H1A O1 H1B 110(3) . . ?
Os1 N1 Os1 180.0 . 3_566 ?
Os1 N2 H2A 109.5 . . ?
Os1 N2 H2B 109.5 . . ?
Os1 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
Os1 N3 H3A 109.5 . . ?
Os1 N3 H3B 109.5 . . ?
Os1 N3 H3C 109.5 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Os1 N4 H4A 109.5 . . ?
Os1 N4 H4B 109.5 . . ?
Os1 N4 H4C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
Os1 N5 H5A 109.5 . . ?
Os1 N5 H5B 109.5 . . ?
Os1 N5 H5C 109.5 . . ?
H5A N5 H5B 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
O4 N11 O5 120.1(3) . . ?
O6 N11 O4 120.8(3) . . ?
O6 N11 O5 119.1(2) . . ?
O13 N14 O14 122.1(3) . . ?
O13 N14 O15 119.9(2) . . ?
O14 N14 O15 118.0(2) . . ?
N6 Os2 O2 179.06(7) . . ?
N6 Os2 N7 97.04(7) . . ?
N6 Os2 N8 95.25(7) . . ?
N6 Os2 N9 95.54(7) . . ?
N6 Os2 N10 92.87(7) . . ?
N7 Os2 O2 82.73(10) . . ?
N7 Os2 N8 88.77(11) . . ?
N7 Os2 N10 89.04(10) . . ?
N8 Os2 O2 83.84(10) . . ?
N9 Os2 O2 84.71(10) . . ?
N9 Os2 N7 167.34(10) . . ?
N9 Os2 N8 91.45(12) . . ?
N9 Os2 N10 88.96(10) . . ?
N10 Os2 O2 88.04(9) . . ?
N10 Os2 N8 171.80(10) . . ?
Os2 O2 H2D 122(3) . . ?
Os2 O2 H2E 127(3) . . ?
H2D O2 H2E 106(4) . . ?
Os2 N6 Os2 180.0 3_656 . ?
Os2 N7 H7A 109.5 . . ?
Os2 N7 H7B 109.5 . . ?
Os2 N7 H7C 109.5 . . ?
H7A N7 H7B 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
Os2 N8 H8A 109.5 . . ?
Os2 N8 H8B 109.5 . . ?
Os2 N8 H8C 109.5 . . ?
H8A N8 H8B 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
Os2 N9 H9A 109.5 . . ?
Os2 N9 H9B 109.5 . . ?
Os2 N9 H9C 109.5 . . ?
H9A N9 H9B 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
Os2 N10 H10A 109.5 . . ?
Os2 N10 H10B 109.5 . . ?
Os2 N10 H10C 109.5 . . ?
H10A N10 H10B 109.5 . . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
H3D O3 H3E 90(6) . . ?
O8 N12 O7 120.5(3) . . ?
O9 N12 O7 119.9(2) . . ?
O9 N12 O8 119.6(3) . . ?
O11 N13 O10 122.3(3) . . ?
O12 N13 O10 117.6(3) . . ?
O12 N13 O11 120.1(3) . . ?
O17 N15 O16 120.5(3) . . ?
O18 N15 O16 118.7(3) . . ?
O18 N15 O17 120.8(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O7 0.839(18) 1.93(2) 2.747(3) 164(4) 2_646
O1 H1B O5 0.845(18) 1.85(2) 2.651(3) 159(4) .
N4 H4C O9 0.91 2.12 2.894(3) 143.0 2_646
O2 H2D O15 0.825(19) 1.87(2) 2.657(3) 160(4) 4_565
O2 H2E O16 0.840(19) 1.79(2) 2.620(3) 168(4) 3_666
N9 H9B O12 0.91 2.26 2.827(4) 120.3 2_646

_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 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.805
