# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_raza_Fehopo_prima_sintesi
_database_code_depnum_ccdc_archive 'CCDC 2520137'
loop_
_audit_author_name
_audit_author_address
'Samuele Ciattini'
;University of Florence
Italy
;
_audit_update_record             
;
2026-01-04 deposited with the CCDC.	2026-03-16 downloaded from the CCDC.
;
_audit_creation_date             2025-10-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7311)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_iupac          ?
_chemical_formula_moiety         '0.667(C21 H24 Fe N3 O6), 8(H2 O)'
_chemical_formula_sum            'C14 H32 Fe0.67 N2 O12'
_chemical_formula_weight         457.65
_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'
Fe Fe 0.3463 0.8444 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   16.5275(3)
_cell_length_b                   16.5275(3)
_cell_length_c                   6.7967(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1607.84(8)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    9420
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      35.5466
_cell_measurement_theta_min      2.4646
_exptl_absorpt_coefficient_mu    0.548
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.6830
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       clear
_exptl_crystal_F_000             730
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
;
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            55277
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         35.64
_diffrn_reflns_theta_min         2.46
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  ?
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              ?
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4221
_reflns_number_total             4944
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.480
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    ?
_refine_ls_number_parameters     153
_refine_ls_number_reflns         4944
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0393
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0536P)²+0.9278P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1088
_refine_special_details          
;
;
_olex2_refinement_description    
;
1. Others
 Fixed X: H1A(0.9458)
 Fixed Y: H1A(0.103703)
 Fixed Z: H1A(1.013)
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.61215(6) 0.21770(6) -0.07028(12) 0.01561(14) Uani d . . . 1 . .
N N1 0.63219(7) 0.01039(6) -0.01812(14) 0.01512(16) Uani d . . . 1 . .
C C1 0.68029(7) 0.17483(7) 0.18206(15) 0.01385(17) Uani d . . . 1 . .
O O2 0.70053(6) 0.25340(6) 0.26689(12) 0.01616(14) Uani d . . . 1 . .
C C2 0.63237(7) 0.15438(7) -0.00159(15) 0.01297(16) Uani d . . . 1 . .
O O3 0.79239(8) 0.27870(7) 0.63019(14) 0.02432(18) Uani d . . . 1 . .
H H1 0.7776(15) 0.3097(16) 0.715(3) 0.036000 Uiso d U . . 1 . .
H H1AA 0.7617(16) 0.2695(15) 0.535(3) 0.036000 Uiso d U . . 1 . .
C C3 0.61003(7) 0.07228(7) -0.10136(15) 0.01386(16) Uani d . . . 1 . .
O O4 0.81791(7) 0.13422(7) 0.73699(14) 0.02256(17) Uani d . . . 1 . .
H H1B 0.8072(15) 0.1750(16) 0.706(3) 0.034000 Uiso d U . . 1 . .
H H1C 0.8412(15) 0.1248(15) 0.644(3) 0.034000 Uiso d U . . 1 . .
C C4 0.56341(9) 0.04977(8) -0.29756(17) 0.0195(2) Uani d . . . 1 . .
H H4A 0.558619 0.103229 -0.344897 0.029000 Uiso calc U . R 1 . .
H H4B 0.500716 -0.004910 -0.285805 0.029000 Uiso calc U . R 1 . .
H H4C 0.600266 0.036207 -0.390909 0.029000 Uiso calc U . R 1 . .
O O5 0.89440(6) 0.08219(6) 1.03333(13) 0.01850(15) Uani d . . . 1 . .
H H1A 0.945800 0.103703 1.013000 0.028000 Uiso d U . . 1 . .
H H1D 0.8714(14) 0.1019(14) 0.970(3) 0.028000 Uiso d U . . 1 . .
C C5 0.61145(9) -0.07602(8) -0.12157(19) 0.0205(2) Uani d . . . 1 . .
H H5A 0.625166 -0.115036 -0.034902 0.031000 Uiso calc U . R 1 . .
H H5B 0.650076 -0.060423 -0.240277 0.031000 Uiso calc U . R 1 . .
H H5C 0.545274 -0.110197 -0.158489 0.031000 Uiso calc U . R 1 . .
Fe Fe1 0.666667 0.333333 0.09369(4) 0.01124(6) Uani d T P S 1 . .
O O6 0.90171(8) 0.08615(8) 1.44103(14) 0.0278(2) Uani d . . . 1 . .
H H1E 0.8946(17) 0.0858(17) 1.339(4) 0.042000 Uiso d U . . 1 . .
H H1F 0.9640(17) 0.1194(17) 1.484(4) 0.042000 Uiso d U . . 1 . .
C C6 0.67768(8) 0.02874(8) 0.15665(17) 0.01727(18) Uani d . . . 1 . .
H H6 0.692377 -0.015512 0.209867 0.021000 Uiso calc U . R 1 . .
C C7 0.70298(8) 0.10967(8) 0.25848(16) 0.01635(18) Uani d . . . 1 . .
H H7 0.735588 0.121544 0.379740 0.020000 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C2 . 1.3320(13) ?
O1 Fe1 . 1.9961(8) ?
N1 C3 . 1.3694(14) ?
N1 C5 . 1.4703(14) ?
N1 C6 . 1.3565(14) ?
C1 O2 . 1.3024(13) ?
C1 C2 . 1.4255(14) ?
C1 C7 . 1.4049(15) ?
O2 Fe1 . 2.0454(8) ?
C2 C3 . 1.3916(14) ?
C3 C4 . 1.4912(15) ?
C6 C7 . 1.3725(16) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 O1 Fe1 . . 112.71(6) ?
C3 N1 C5 . . 120.56(10) ?
C6 N1 C3 . . 121.33(9) ?
C6 N1 C5 . . 118.04(10) ?
O2 C1 C2 . . 117.34(9) ?
O2 C1 C7 . . 124.52(9) ?
C7 C1 C2 . . 118.14(9) ?
C1 O2 Fe1 . . 111.87(6) ?
O1 C2 C1 . . 116.65(9) ?
O1 C2 C3 . . 123.15(9) ?
C3 C2 C1 . . 120.19(9) ?
N1 C3 C2 . . 119.17(9) ?
N1 C3 C4 . . 118.75(9) ?
C2 C3 C4 . . 122.07(10) ?
O1 Fe1 O1 3_665 . 91.86(3) ?
O1 Fe1 O1 . 2_655 91.86(3) ?
O1 Fe1 O1 3_665 2_655 91.86(3) ?
O1 Fe1 O2 3_665 . 167.56(3) ?
O1 Fe1 O2 . 2_655 167.56(3) ?
O1 Fe1 O2 . 3_665 98.41(3) ?
O1 Fe1 O2 . . 80.86(3) ?
O1 Fe1 O2 3_665 3_665 80.86(3) ?
O1 Fe1 O2 2_655 . 98.41(3) ?
O1 Fe1 O2 2_655 3_665 167.56(3) ?
O1 Fe1 O2 3_665 2_655 98.41(3) ?
O1 Fe1 O2 2_655 2_655 80.86(3) ?
O2 Fe1 O2 . 3_665 90.18(3) ?
O2 Fe1 O2 2_655 3_665 90.18(3) ?
O2 Fe1 O2 . 2_655 90.18(3) ?
N1 C6 C7 . . 121.62(10) ?
C6 C7 C1 . . 119.51(10) ?

_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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2521079'
loop_
_audit_author_name
_audit_author_address
'Samuele Ciattini'
;University of Florence
Italy
;
_audit_update_record             
;
2026-01-07 deposited with the CCDC.	2026-03-16 downloaded from the CCDC.
;
_audit_creation_date             2026-01-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7311)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C7 H8 N O2 Ru0.333, 4(H2 O)'
_chemical_formula_sum            'C7 H16 N O6 Ru0.33'
_chemical_formula_weight         243.90
_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      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   16.6350(3)
_cell_length_b                   16.6350(3)
_cell_length_c                   6.7695(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1622.31(8)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.45
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.798
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.102
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            48453
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_min         2.449
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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                2484
_reflns_number_total             2694
_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 V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       APEX5V2022.8-RC126
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'XT, VERSION 2018/2'
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2694
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0312
_refine_ls_restrained_S_all      1.051
_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)+(0.0304P)²+2.0945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0765
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB = O2W-H2WA = O2W-H2WB
 0.82 with sigma of 0.001
 O3W-H3WA = O3W-H3WB = O4W-H4WA = O4W-H4WB
 0.82 with sigma of 0.001
 H1WA-H1WB = H2WA-H2WB = H3WA-H3WB = H4WA-H4WB
 1.31 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.333333 0.666667 0.90571(4) 0.01362(8) Uani 1 3 d S T P . .
O1 O 0.28998(10) 0.74148(10) 0.7405(2) 0.0210(3) Uani 1 1 d . . . . .
O2 O 0.39199(10) 0.78396(10) 1.0714(2) 0.0211(3) Uani 1 1 d . . . . .
N1 N 0.36668(11) 0.98675(11) 1.0199(2) 0.0171(3) Uani 1 1 d . . . . .
C1 C 0.31493(13) 0.82122(13) 0.8239(3) 0.0182(4) Uani 1 1 d . . . . .
C2 C 0.29212(14) 0.88608(14) 0.7481(3) 0.0211(4) Uani 1 1 d . . . . .
H2 H 0.258785 0.873735 0.630935 0.025 Uiso 1 1 calc R U . . .
C3 C 0.31901(14) 0.96709(14) 0.8469(3) 0.0214(4) Uani 1 1 d . . . . .
H3 H 0.304379 1.009901 0.794684 0.026 Uiso 1 1 calc R U . . .
C4 C 0.38745(15) 1.07301(14) 1.1231(3) 0.0252(4) Uani 1 1 d . . . . .
H4A H 0.452757 1.108554 1.150449 0.038 Uiso 1 1 calc R U . . .
H4B H 0.353420 1.057978 1.244965 0.038 Uiso 1 1 calc R U . . .
H4C H 0.369714 1.108693 1.041288 0.038 Uiso 1 1 calc R U . . .
C5 C 0.39084(13) 0.92662(13) 1.1001(3) 0.0186(4) Uani 1 1 d . . . . .
C6 C 0.43949(15) 0.94978(15) 1.2940(3) 0.0246(4) Uani 1 1 d . . . . .
H6A H 0.453131 0.902053 1.330157 0.037 Uiso 1 1 calc R U . . .
H6B H 0.400447 0.954122 1.392861 0.037 Uiso 1 1 calc R U . . .
H6C H 0.496286 1.008096 1.284192 0.037 Uiso 1 1 calc R U . . .
C7 C 0.36752(13) 0.84400(13) 1.0010(3) 0.0168(4) Uani 1 1 d . . . . .
O1W O 0.20756(12) 0.72330(12) 0.3689(2) 0.0302(4) Uani 1 1 d D . . . .
H1WA H 0.2392(14) 0.7304(18) 0.467(2) 0.036 Uiso 1 1 d D U . . .
H1WB H 0.2208(15) 0.6950(15) 0.288(2) 0.036 Uiso 1 1 d D U . . .
O2W O 0.17994(12) 0.86518(12) 0.2600(2) 0.0271(3) Uani 1 1 d D . . . .
H2WA H 0.1908(15) 0.8237(11) 0.289(3) 0.033 Uiso 1 1 d D U . . .
H2WB H 0.1590(16) 0.8754(16) 0.3606(18) 0.033 Uiso 1 1 d D U . . .
O3W O 0.10407(10) 0.91762(10) -0.0335(2) 0.0199(3) Uani 1 1 d D . . . .
H3WA H 0.1321(11) 0.9018(14) 0.042(3) 0.024 Uiso 1 1 d D U . . .
H3WB H 0.0496(4) 0.8894(15) 0.002(3) 0.024 Uiso 1 1 d D U . . .
O4W O 0.09855(12) 0.91498(13) -0.4417(2) 0.0308(4) Uani 1 1 d D . . . .
H4WA H 0.1011(16) 0.9134(19) -0.3209(4) 0.037 Uiso 1 1 d D U . . .
H4WB H 0.0433(4) 0.8868(18) -0.471(3) 0.037 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 O1 2.0537(14) 2_665 ?
Ru1 O1 2.0537(14) 3_565 ?
Ru1 O1 2.0537(14) . ?
Ru1 O2 2.0283(14) . ?
Ru1 O2 2.0283(14) 3_565 ?
Ru1 O2 2.0283(14) 2_665 ?
O1 C1 1.304(2) . ?
O2 C7 1.341(2) . ?
N1 C3 1.359(3) . ?
N1 C4 1.474(2) . ?
N1 C5 1.364(3) . ?
C1 C2 1.407(3) . ?
C1 C7 1.420(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.364(3) . ?
C3 H3 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.488(3) . ?
C5 C7 1.399(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
O1W H1WA 0.8200(10) . ?
O1W H1WB 0.8200(10) . ?
O2W H2WA 0.8200(10) . ?
O2W H2WB 0.8200(10) . ?
O3W H3WA 0.8199(10) . ?
O3W H3WB 0.8199(10) . ?
O4W H4WA 0.8199(10) . ?
O4W H4WB 0.8200(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ru1 O1 93.16(6) 2_665 3_565 ?
O1 Ru1 O1 93.16(6) . 2_665 ?
O1 Ru1 O1 93.16(6) . 3_565 ?
O2 Ru1 O1 82.19(6) 2_665 2_665 ?
O2 Ru1 O1 172.68(6) 2_665 3_565 ?
O2 Ru1 O1 172.68(6) 3_565 . ?
O2 Ru1 O1 92.74(6) . 3_565 ?
O2 Ru1 O1 82.19(6) . . ?
O2 Ru1 O1 92.74(6) 2_665 . ?
O2 Ru1 O1 92.74(6) 3_565 2_665 ?
O2 Ru1 O1 172.68(6) . 2_665 ?
O2 Ru1 O1 82.19(6) 3_565 3_565 ?
O2 Ru1 O2 92.35(6) 3_565 . ?
O2 Ru1 O2 92.35(6) 2_665 3_565 ?
O2 Ru1 O2 92.35(6) 2_665 . ?
C1 O1 Ru1 110.55(12) . . ?
C7 O2 Ru1 109.92(12) . . ?
C3 N1 C4 117.88(17) . . ?
C3 N1 C5 121.14(17) . . ?
C5 N1 C4 120.92(17) . . ?
O1 C1 C2 123.46(18) . . ?
O1 C1 C7 118.53(17) . . ?
C2 C1 C7 118.01(18) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.84(18) . . ?
C3 C2 H2 120.1 . . ?
N1 C3 C2 121.59(18) . . ?
N1 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 118.88(17) . . ?
N1 C5 C7 119.42(18) . . ?
C7 C5 C6 121.68(18) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O2 C7 C1 118.53(17) . . ?
O2 C7 C5 121.55(17) . . ?
C5 C7 C1 119.91(18) . . ?
H1WA O1W H1WB 106.5(11) . . ?
H2WA O2W H2WB 105.8(11) . . ?
H3WA O3W H3WB 106.1(11) . . ?
H4WA O4W H4WB 106.4(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ru1 O1 C1 C2 -177.72(15) . . . . ?
Ru1 O1 C1 C7 2.0(2) . . . . ?
Ru1 O2 C7 C1 -5.1(2) . . . . ?
Ru1 O2 C7 C5 173.43(14) . . . . ?
O1 C1 C2 C3 178.42(19) . . . . ?
O1 C1 C7 O2 2.2(3) . . . . ?
O1 C1 C7 C5 -176.36(17) . . . . ?
N1 C5 C7 O2 178.18(17) . . . . ?
N1 C5 C7 C1 -3.3(3) . . . . ?
C1 C2 C3 N1 -0.9(3) . . . . ?
C2 C1 C7 O2 -178.07(17) . . . . ?
C2 C1 C7 C5 3.3(3) . . . . ?
C3 N1 C5 C6 -177.43(18) . . . . ?
C3 N1 C5 C7 1.1(3) . . . . ?
C4 N1 C3 C2 -176.00(19) . . . . ?
C4 N1 C5 C6 -0.5(3) . . . . ?
C4 N1 C5 C7 178.04(17) . . . . ?
C5 N1 C3 C2 1.0(3) . . . . ?
C6 C5 C7 O2 -3.3(3) . . . . ?
C6 C5 C7 C1 175.20(18) . . . . ?
C7 C1 C2 C3 -1.3(3) . . . . ?

_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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2520138'
loop_
_audit_author_name
_audit_author_address
'Samuele Ciattini'
;University of Florence
Italy
;
_audit_update_record             
;
2026-01-04 deposited with the CCDC.	2026-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H19 Cl4 N3 O2 Os'
_chemical_formula_weight         641.36

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   12.3716(7)
_cell_length_b                   8.8491(6)
_cell_length_c                   20.2098(14)
_cell_angle_alpha                90
_cell_angle_beta                 99.749(2)
_cell_angle_gamma                90
_cell_volume                     2180.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9233
_cell_measurement_theta_min      2.4116
_cell_measurement_theta_max      30.5683

_exptl_crystal_description       prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.173
_exptl_absorpt_coefficient_mu    6.357
_shelx_estimated_absorpt_T_min   0.277
_shelx_estimated_absorpt_T_max   0.406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3106
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_source                   ?
_diffrn_detector_area_resol_mean 7.3910
_diffrn_source_power             0.07
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_reflns_number            55707
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.412
_diffrn_reflns_theta_max         30.623
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6707
_reflns_number_gt                6214
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       APEX5V2022.8-RC126
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0269P)²+23.8052P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6707
_refine_ls_number_parameters     281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0974
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Os1 Os 0.24789(2) 0.43900(2) 0.22444(2) 0.01281(6) Uani 1 1 d . . . . .
Cl1 Cl 0.39644(9) 0.51977(14) 0.17370(6) 0.0178(2) Uani 1 1 d . . . . .
Cl2 Cl 0.11682(10) 0.49969(15) 0.12791(6) 0.0198(2) Uani 1 1 d . . . . .
O1 O 0.3475(3) 0.3823(4) 0.31191(17) 0.0160(6) Uani 1 1 d . . . . .
O2 O 0.1297(3) 0.3654(4) 0.27743(18) 0.0175(7) Uani 1 1 d . . . . .
N1 N 0.2630(3) 0.2170(4) 0.1918(2) 0.0162(8) Uani 1 1 d . . . . .
N2 N 0.2343(3) 0.6512(4) 0.2665(2) 0.0139(7) Uani 1 1 d . . . . .
N3 N 0.2729(4) 0.2448(5) 0.4660(2) 0.0213(9) Uani 1 1 d . . . . .
C1 C 0.1769(4) 0.1388(6) 0.1600(3) 0.0211(10) Uani 1 1 d . . . . .
H1 H 0.106729 0.185502 0.152131 0.025 Uiso 1 1 calc R U . . .
C2 C 0.1871(5) -0.0072(6) 0.1384(3) 0.0249(11) Uani 1 1 d . . . . .
H2 H 0.124428 -0.059484 0.115877 0.030 Uiso 1 1 calc R U . . .
C3 C 0.2887(5) -0.0785(6) 0.1493(3) 0.0239(11) Uani 1 1 d . . . . .
H3 H 0.296927 -0.179111 0.134593 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3783(4) 0.0034(6) 0.1828(3) 0.0205(10) Uani 1 1 d . . . . .
H4 H 0.449315 -0.040704 0.191172 0.025 Uiso 1 1 calc R U . . .
C5 C 0.3620(4) 0.1490(6) 0.2034(3) 0.0174(9) Uani 1 1 d . . . . .
H5 H 0.422952 0.203572 0.226687 0.021 Uiso 1 1 calc R U . . .
C6 C 0.3253(4) 0.7221(6) 0.2967(3) 0.0195(9) Uani 1 1 d . . . . .
H6 H 0.394165 0.673922 0.297827 0.023 Uiso 1 1 calc R U . . .
C7 C 0.3225(4) 0.8638(6) 0.3265(3) 0.0231(10) Uani 1 1 d . . . . .
H8 H 0.388398 0.912112 0.346804 0.028 Uiso 1 1 calc R U . . .
C8 C 0.2217(5) 0.9328(6) 0.3261(3) 0.0245(11) Uani 1 1 d . . . . .
H9 H 0.216902 1.029081 0.346142 0.029 Uiso 1 1 calc R U . . .
C9 C 0.1281(4) 0.8574(6) 0.2955(3) 0.0229(10) Uani 1 1 d . . . . .
H10 H 0.058041 0.901855 0.294756 0.027 Uiso 1 1 calc R U . . .
C10 C 0.1367(4) 0.7174(5) 0.2661(3) 0.0171(9) Uani 1 1 d . . . . .
H11 H 0.071974 0.667178 0.245163 0.021 Uiso 1 1 calc R U . . .
C11 C 0.2889(4) 0.3372(5) 0.3577(2) 0.0162(9) Uani 1 1 d . . . . .
C12 C 0.1719(4) 0.3282(5) 0.3386(2) 0.0162(8) Uani 1 1 d . . . . .
C13 C 0.1105(4) 0.2756(5) 0.3860(3) 0.0184(9) Uani 1 1 d . . . . .
H15 H 0.032962 0.267885 0.374818 0.022 Uiso 1 1 calc R U . . .
C14 C 0.1634(5) 0.2353(6) 0.4489(3) 0.0240(11) Uani 1 1 d . . . . .
H16 H 0.121492 0.199903 0.481057 0.029 Uiso 1 1 calc R U . . .
C15 C 0.3246(6) 0.2013(9) 0.5354(3) 0.0378(15) Uani 1 1 d . . . . .
H17A H 0.404305 0.213964 0.540525 0.057 Uiso 1 1 calc R U . . .
H17B H 0.296056 0.265958 0.567865 0.057 Uiso 1 1 calc R U . . .
H17C H 0.307509 0.095503 0.543514 0.057 Uiso 1 1 calc R U . . .
C16 C 0.3383(4) 0.2938(6) 0.4215(3) 0.0198(9) Uani 1 1 d . . . . .
C17 C 0.4599(5) 0.2989(8) 0.4418(3) 0.0299(12) Uani 1 1 d . . . . .
H19A H 0.493113 0.336332 0.404263 0.045 Uiso 1 1 calc R U . . .
H19B H 0.478990 0.366681 0.480396 0.045 Uiso 1 1 calc R U . . .
H19C H 0.487476 0.197184 0.454144 0.045 Uiso 1 1 calc R U . . .
Cl3A Cl 0.0868(5) 0.6294(5) 0.4561(3) 0.0563(14) Uani 0.644(8) 1 d . . P A 1
Cl4A Cl 0.2769(2) 0.8228(4) 0.49281(14) 0.0455(11) Uani 0.644(8) 1 d . . P A 1
C18A C 0.1334(11) 0.8159(15) 0.4741(7) 0.027(2) Uani 0.644(8) 1 d . . P A 1
H6A H 0.107304 0.881471 0.434986 0.032 Uiso 0.644(8) 1 calc R U P A 1
H6B H 0.102284 0.854874 0.512818 0.032 Uiso 0.644(8) 1 calc R U P A 1
Cl4B Cl 0.2849(5) 0.6717(15) 0.4739(3) 0.084(4) Uani 0.356(8) 1 d . . P A 2
C18B C 0.167(3) 0.773(3) 0.4832(18) 0.051(9) Uani 0.356(8) 1 d . . P A 2
H77A H 0.177711 0.821194 0.527969 0.061 Uiso 0.356(8) 1 calc R U P A 2
H77B H 0.153527 0.853060 0.448736 0.061 Uiso 0.356(8) 1 calc R U P A 2
Cl3B Cl 0.0565(7) 0.6538(15) 0.4750(6) 0.062(3) Uani 0.356(8) 1 d . . P A 2


_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 2.039(3) . ?
Os1 O2 2.059(3) . ?
Os1 N2 2.080(4) . ?
Os1 N1 2.091(4) . ?
Os1 Cl1 2.3618(12) . ?
Os1 Cl2 2.3775(12) . ?
O1 C11 1.331(6) . ?
O2 C12 1.300(6) . ?
N1 C1 1.340(6) . ?
N1 C5 1.349(6) . ?
N2 C10 1.340(6) . ?
N2 C6 1.342(6) . ?
N3 C14 1.343(7) . ?
N3 C16 1.376(7) . ?
N3 C15 1.491(7) . ?
C1 C2 1.377(8) . ?
C2 C3 1.390(8) . ?
C3 C4 1.399(8) . ?
C4 C5 1.380(7) . ?
C6 C7 1.394(7) . ?
C7 C8 1.387(8) . ?
C8 C9 1.387(8) . ?
C9 C10 1.386(7) . ?
C11 C16 1.385(7) . ?
C11 C12 1.435(7) . ?
C12 C13 1.400(7) . ?
C13 C14 1.375(8) . ?
C16 C17 1.492(8) . ?
Cl3A C18A 1.765(14) . ?
Cl4A C18A 1.754(14) . ?
Cl4B C18B 1.75(3) . ?
C18B Cl3B 1.71(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Os1 O2 81.35(14) . . ?
O1 Os1 N2 86.95(15) . . ?
O2 Os1 N2 87.66(14) . . ?
O1 Os1 N1 88.22(15) . . ?
O2 Os1 N1 88.64(16) . . ?
N2 Os1 N1 174.31(16) . . ?
O1 Os1 Cl1 92.88(10) . . ?
O2 Os1 Cl1 174.22(11) . . ?
N2 Os1 Cl1 91.55(11) . . ?
N1 Os1 Cl1 91.70(13) . . ?
O1 Os1 Cl2 174.33(10) . . ?
O2 Os1 Cl2 93.00(11) . . ?
N2 Os1 Cl2 92.31(12) . . ?
N1 Os1 Cl2 92.20(12) . . ?
Cl1 Os1 Cl2 92.76(4) . . ?
C11 O1 Os1 110.9(3) . . ?
C12 O2 Os1 111.6(3) . . ?
C1 N1 C5 118.6(4) . . ?
C1 N1 Os1 122.0(3) . . ?
C5 N1 Os1 119.4(3) . . ?
C10 N2 C6 118.9(4) . . ?
C10 N2 Os1 121.8(3) . . ?
C6 N2 Os1 119.2(3) . . ?
C14 N3 C16 122.1(5) . . ?
C14 N3 C15 118.6(5) . . ?
C16 N3 C15 119.3(5) . . ?
N1 C1 C2 121.9(5) . . ?
C1 C2 C3 120.3(5) . . ?
C2 C3 C4 117.6(5) . . ?
C5 C4 C3 119.0(5) . . ?
N1 C5 C4 122.6(5) . . ?
N2 C6 C7 122.5(5) . . ?
C8 C7 C6 118.7(5) . . ?
C7 C8 C9 118.2(5) . . ?
C10 C9 C8 120.1(5) . . ?
N2 C10 C9 121.5(5) . . ?
O1 C11 C16 121.6(5) . . ?
O1 C11 C12 118.2(4) . . ?
C16 C11 C12 120.1(5) . . ?
O2 C12 C13 123.9(5) . . ?
O2 C12 C11 117.8(4) . . ?
C13 C12 C11 118.3(4) . . ?
C14 C13 C12 119.4(5) . . ?
N3 C14 C13 121.5(5) . . ?
N3 C16 C11 118.7(5) . . ?
N3 C16 C17 120.5(5) . . ?
C11 C16 C17 120.9(5) . . ?
Cl4A C18A Cl3A 111.1(8) . . ?
Cl3B C18B Cl4B 110.1(16) . . ?

_refine_diff_density_max         2.082
_refine_diff_density_min         -3.066
_refine_diff_density_rms         0.220



####################################################################### 
# 
# 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_exp_725_v67
_database_code_depnum_ccdc_archive 'CCDC 2520606'
loop_
_audit_author_name
_audit_author_address
'Jesper Bendix'
;University of Copenhagen
Denmark
;
_audit_update_record             
;
2026-01-05 deposited with the CCDC.	2026-03-16 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT084_exp_725_v67         
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.46 Report
RESPONSE: High wR2 arises from refinement against 3D electron diffraction data.
;
_vrf_PLAT306_exp_725_v67         
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O2 Check
RESPONSE: O2 corresponds to a [hydroxyl / water / solvent] oxygen. Hydrogen atoms could not be determined from the diffraction experiment
;
# Added during the CSD deposition process: Monday 05 January 2026 08:56 PM
# end Validation Reply Form

_chemical_oxdiff_formula         'C7 H8 N1 O1 Na0.330 S1 Ru0.330 '
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     0.90
_reflns_odcompleteness_completeness 99.89
_diffrn_oxdiff_scatteringfactors_ed 
;
UCLA (2022) https://srv.mbi.ucla.edu/faes/data
;
_diffrn_oxdiff_digest_creation   'CAP 1.171.44.66a, AC 1.5-ac7-004'
_diffrn_oxdiff_digest_hkl        4370d4cba1ccde0976ab299b7d1d308df4ae5e
_diffrn_orient_matrix_UB_33      -0.0001118000
_diffrn_orient_matrix_UB_32      -0.0006853000
_diffrn_orient_matrix_UB_31      -0.0020148000
_diffrn_orient_matrix_UB_23      -0.0005276000
_diffrn_orient_matrix_UB_22      0.0009909000
_diffrn_orient_matrix_UB_21      0.0005117000
_diffrn_orient_matrix_UB_13      0.0002634000
_diffrn_orient_matrix_UB_12      0.0016938000
_diffrn_orient_matrix_UB_11      0.0001693000
_diffrn_orient_matrix_type       
;
CrysAlisPro convention (1999,Acta A55,543-557)
;
_oxdiff_exptl_crystal_thickness  1000.0
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.054
_oxdiff_exptl_absorpt_empirical_full_min 0.700
_cell_oxdiff_measurement_reflns_used 935
_cell_oxdiff_volume              7025(2)
_cell_oxdiff_angle_gamma         120.11(2)
_cell_oxdiff_angle_beta          89.996(9)
_cell_oxdiff_angle_alpha         89.999(11)
_cell_oxdiff_length_c            41.819(3)
_cell_oxdiff_length_b            13.958(3)
_cell_oxdiff_length_a            13.911(2)
_audit_creation_date             2024-09-02
_audit_creation_method           
;
FinalCif V142 by Daniel Kratzert, Freiburg 2024,
https://dkratzert.de/finalcif.html
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_sum            'C42 H49 N6 Na O7 Ru2 S6'
_chemical_formula_moiety         'C42 H48 N6 Na O6 Ru2 S6, OH'
_chemical_formula_weight         1167.42
_chemical_melting_point          ?
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   13.922(3)
_cell_length_b                   13.922(3)
_cell_length_c                   41.850(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7025(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    934
_cell_measurement_theta_min      0.0690
_cell_measurement_theta_max      0.7720
_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_F_000             1279
_exptl_crystal_size_max          0.0013
_exptl_crystal_size_mid          0.00052
_exptl_crystal_size_min          0.0002
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.44.66a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_special_details           ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_radiation_monochromator  none
_diffrn_measurement_ambient_temperature_device_make ?
_diffrn_radiation_probe          electron
_diffrn_source                   'electron diffractometer'
_diffrn_source_type              'JEOL JSM-2300ED, LaB6'
_diffrn_source_voltage           200
_diffrn_source_current           ?
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix-ED
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
;
XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV
;
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_measurement_specimen_support ?
_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  54.00   0.25    1.00    --    0.00   0.00   0.00  484
;
_diffrn_reflns_number            8760
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_av_R_equivalents  0.1244
_diffrn_reflns_av_sigmaI/netI    0.2088
_diffrn_reflns_theta_min         0.069
_diffrn_reflns_theta_max         0.836
_diffrn_reflns_theta_full        0.836
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1299
_reflns_number_gt                737
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       
;
CrysAlisPro system (CCD 43.128a 64-bit (release 20-06-2024))
;
_computing_cell_refinement       'CrysAlisPro 1.171.44.66a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.44.66a (Rigaku OD, 2024)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
w=1/[σ²(Fo²)+(0.2483P)²+8.4600P] where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         1299
_refine_ls_number_parameters     101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2048
_refine_ls_R_factor_gt           0.1492
_refine_ls_wR_factor_ref         0.4598
_refine_ls_wR_factor_gt          0.4222
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       11(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_
_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 0.666667 0.333333 0.51135(8) 0.0510(16) Uani 1 3 d S T P . .
S1 S 0.6186(6) 0.4406(5) 0.48161(11) 0.072(2) Uani 1 1 d . . . . .
Na1 Na 0.666667 0.333333 0.583333 0.055(5) Uani 1 6 d S T P . .
O1 O 0.7401(9) 0.4721(10) 0.5420(2) 0.063(3) Uani 1 1 d . . . . .
N1 N 0.7688(12) 0.7431(11) 0.5446(3) 0.082(4) Uani 1 1 d . . . . .
C1 C 0.6750(11) 0.5560(11) 0.5048(2) 0.066(4) Uani 1 1 d . . . . .
C2 C 0.7319(9) 0.5591(10) 0.5340(2) 0.053(3) Uani 1 1 d . . . . .
C3 C 0.7801(10) 0.6538(11) 0.5534(3) 0.060(3) Uani 1 1 d . . . . .
C4 C 0.7161(13) 0.7410(12) 0.5172(3) 0.085(4) Uani 1 1 d . . . . .
H4 H 0.712495 0.813987 0.510232 0.102 Uiso 1 1 calc R U . . .
C5 C 0.6687(12) 0.6514(12) 0.4986(3) 0.082(5) Uani 1 1 d . . . . .
H5 H 0.623311 0.652515 0.477701 0.098 Uiso 1 1 calc R U . . .
C6 C 0.8376(13) 0.6557(12) 0.5837(3) 0.081(4) Uani 1 1 d . . . . .
H6A H 0.821086 0.573179 0.589072 0.121 Uiso 1 1 calc R U . . .
H6B H 0.807511 0.685170 0.602838 0.121 Uiso 1 1 calc R U . . .
H6C H 0.925581 0.710098 0.580922 0.121 Uiso 1 1 calc R U . . .
C7 C 0.8178(16) 0.8441(14) 0.5637(4) 0.112(6) Uani 1 1 d . . . . .
H7A H 0.788582 0.824119 0.587963 0.168 Uiso 1 1 calc R U . . .
H7B H 0.794225 0.900960 0.553945 0.168 Uiso 1 1 calc R U . . .
H7C H 0.906771 0.881984 0.563334 0.168 Uiso 1 1 calc R U . . .
O2 O 1.000000 1.000000 0.500000 0.064(7) Uani 1 6 d S T P . .


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 O1 2.109(10) . ?
Ru1 O1 2.109(10) 3_665 ?
Ru1 O1 2.109(10) 2_655 ?
Ru1 S1 2.286(6) 2_655 ?
Ru1 S1 2.286(6) 3_665 ?
Ru1 S1 2.286(6) . ?
Ru1 Na1 3.013(3) . ?
S1 C1 1.697(14) . ?
Na1 O1 2.408(10) 18_655 ?
Na1 O1 2.408(10) 16_545 ?
Na1 O1 2.408(10) 17 ?
Na1 O1 2.408(10) 3_665 ?
Na1 O1 2.408(10) 2_655 ?
Na1 O1 2.408(10) . ?
O1 C2 1.315(15) . ?
N1 C4 1.353(17) . ?
N1 C3 1.379(18) . ?
N1 C7 1.457(19) . ?
C1 C5 1.398(17) . ?
C1 C2 1.445(14) . ?
C2 C3 1.399(16) . ?
C3 C6 1.492(15) . ?
C4 C5 1.332(18) . ?
C4 H4 1.0830 . ?
C5 H5 1.0830 . ?
C6 H6A 1.0770 . ?
C6 H6B 1.0770 . ?
C6 H6C 1.0770 . ?
C7 H7A 1.0770 . ?
C7 H7B 1.0770 . ?
C7 H7C 1.0770 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ru1 O1 86.9(4) . 3_665 ?
O1 Ru1 O1 86.9(4) . 2_655 ?
O1 Ru1 O1 86.9(4) 3_665 2_655 ?
O1 Ru1 S1 170.4(3) . 2_655 ?
O1 Ru1 S1 96.2(3) 3_665 2_655 ?
O1 Ru1 S1 84.2(3) 2_655 2_655 ?
O1 Ru1 S1 96.2(3) . 3_665 ?
O1 Ru1 S1 84.2(3) 3_665 3_665 ?
O1 Ru1 S1 170.4(3) 2_655 3_665 ?
S1 Ru1 S1 93.2(2) 2_655 3_665 ?
O1 Ru1 S1 84.2(3) . . ?
O1 Ru1 S1 170.4(3) 3_665 . ?
O1 Ru1 S1 96.2(3) 2_655 . ?
S1 Ru1 S1 93.2(2) 2_655 . ?
S1 Ru1 S1 93.2(2) 3_665 . ?
O1 Ru1 Na1 52.6(3) . . ?
O1 Ru1 Na1 52.6(3) 3_665 . ?
O1 Ru1 Na1 52.6(3) 2_655 . ?
S1 Ru1 Na1 122.98(16) 2_655 . ?
S1 Ru1 Na1 122.98(16) 3_665 . ?
S1 Ru1 Na1 122.98(16) . . ?
C1 S1 Ru1 99.2(4) . . ?
O1 Na1 O1 74.1(4) 18_655 16_545 ?
O1 Na1 O1 74.1(4) 18_655 17 ?
O1 Na1 O1 74.1(4) 16_545 17 ?
O1 Na1 O1 177.3(5) 18_655 3_665 ?
O1 Na1 O1 107.7(5) 16_545 3_665 ?
O1 Na1 O1 104.3(5) 17 3_665 ?
O1 Na1 O1 104.3(5) 18_655 2_655 ?
O1 Na1 O1 177.3(5) 16_545 2_655 ?
O1 Na1 O1 107.7(5) 17 2_655 ?
O1 Na1 O1 74.1(4) 3_665 2_655 ?
O1 Na1 O1 107.7(5) 18_655 . ?
O1 Na1 O1 104.3(5) 16_545 . ?
O1 Na1 O1 177.3(5) 17 . ?
O1 Na1 O1 74.1(4) 3_665 . ?
O1 Na1 O1 74.1(4) 2_655 . ?
O1 Na1 Ru1 135.9(2) 18_655 . ?
O1 Na1 Ru1 135.9(2) 16_545 . ?
O1 Na1 Ru1 135.9(2) 17 . ?
O1 Na1 Ru1 44.1(2) 3_665 . ?
O1 Na1 Ru1 44.1(2) 2_655 . ?
O1 Na1 Ru1 44.1(2) . . ?
O1 Na1 Ru1 44.1(2) 18_655 16_545 ?
O1 Na1 Ru1 44.1(2) 16_545 16_545 ?
O1 Na1 Ru1 44.1(2) 17 16_545 ?
O1 Na1 Ru1 135.9(2) 3_665 16_545 ?
O1 Na1 Ru1 135.9(2) 2_655 16_545 ?
O1 Na1 Ru1 135.9(2) . 16_545 ?
Ru1 Na1 Ru1 180.0 . 16_545 ?
C2 O1 Ru1 117.7(7) . . ?
C2 O1 Na1 136.3(8) . . ?
Ru1 O1 Na1 83.4(4) . . ?
C4 N1 C3 120.7(12) . . ?
C4 N1 C7 118.2(14) . . ?
C3 N1 C7 121.0(12) . . ?
C5 C1 C2 115.1(11) . . ?
C5 C1 S1 125.0(9) . . ?
C2 C1 S1 119.9(10) . . ?
O1 C2 C3 120.0(10) . . ?
O1 C2 C1 119.0(11) . . ?
C3 C2 C1 121.0(12) . . ?
N1 C3 C2 118.6(10) . . ?
N1 C3 C6 120.8(12) . . ?
C2 C3 C6 120.6(12) . . ?
C5 C4 N1 121.7(13) . . ?
C5 C4 H4 119.1 . . ?
N1 C4 H4 119.1 . . ?
C4 C5 C1 122.8(12) . . ?
C4 C5 H5 118.6 . . ?
C1 C5 H5 118.6 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ru1 S1 C1 C5 -178.3(11) . . . . ?
Ru1 S1 C1 C2 -0.3(10) . . . . ?
Ru1 O1 C2 C3 -179.4(8) . . . . ?
Na1 O1 C2 C3 69.5(16) . . . . ?
Ru1 O1 C2 C1 -0.9(14) . . . . ?
Na1 O1 C2 C1 -112.0(11) . . . . ?
C5 C1 C2 O1 179.0(11) . . . . ?
S1 C1 C2 O1 0.8(16) . . . . ?
C5 C1 C2 C3 -2.6(17) . . . . ?
S1 C1 C2 C3 179.3(9) . . . . ?
C4 N1 C3 C2 -3(2) . . . . ?
C7 N1 C3 C2 -179.6(13) . . . . ?
C4 N1 C3 C6 -179.7(13) . . . . ?
C7 N1 C3 C6 3(2) . . . . ?
O1 C2 C3 N1 -179.1(11) . . . . ?
C1 C2 C3 N1 2.4(17) . . . . ?
O1 C2 C3 C6 -2.2(18) . . . . ?
C1 C2 C3 C6 179.3(11) . . . . ?
C3 N1 C4 C5 3(2) . . . . ?
C7 N1 C4 C5 -179.6(14) . . . . ?
N1 C4 C5 C1 -4(2) . . . . ?
C2 C1 C5 C4 3(2) . . . . ?
S1 C1 C5 C4 -178.7(12) . . . . ?

loop_
_diffrn_frame_id
_diffrn_frame_h
_diffrn_frame_k
_diffrn_frame_l
_diffrn_frame_start_angle
_diffrn_frame_end_angle
_diffrn_frame_scale
1 -0.05340 -0.00846 1.00000 -67.000 -66.750 1.000
2 -0.05390 -0.00699 1.00000 -66.750 -66.500 1.000
3 -0.05440 -0.00553 1.00000 -66.500 -66.250 0.493
4 -0.05491 -0.00407 1.00000 -66.250 -66.000 0.494
5 -0.05541 -0.00260 1.00000 -66.000 -65.750 0.503
6 -0.05591 -0.00114 1.00000 -65.750 -65.500 0.510
7 -0.05641 0.00032 1.00000 -65.500 -65.250 0.513
8 -0.05691 0.00178 1.00000 -65.250 -65.000 0.511
9 -0.05741 0.00324 1.00000 -65.000 -64.750 0.522
10 -0.05791 0.00470 1.00000 -64.750 -64.500 0.525
11 -0.05841 0.00616 1.00000 -64.500 -64.250 0.517
12 -0.05891 0.00762 1.00000 -64.250 -64.000 0.518
13 -0.05941 0.00908 1.00000 -64.000 -63.750 0.525
14 -0.05991 0.01054 1.00000 -63.750 -63.500 0.525
15 -0.06042 0.01200 1.00000 -63.500 -63.250 0.530
16 -0.06092 0.01346 1.00000 -63.250 -63.000 0.545
17 -0.06142 0.01492 1.00000 -63.000 -62.750 0.540
18 -0.06192 0.01638 1.00000 -62.750 -62.500 0.541
19 -0.06242 0.01784 1.00000 -62.500 -62.250 0.537
20 -0.06292 0.01930 1.00000 -62.250 -62.000 0.558
21 -0.06342 0.02076 1.00000 -62.000 -61.750 0.541
22 -0.06392 0.02222 1.00000 -61.750 -61.500 0.555
23 -0.06442 0.02368 1.00000 -61.500 -61.250 0.554
24 -0.06492 0.02514 1.00000 -61.250 -61.000 0.577
25 -0.06542 0.02660 1.00000 -61.000 -60.750 0.566
26 -0.06592 0.02807 1.00000 -60.750 -60.500 0.576
27 -0.06643 0.02953 1.00000 -60.500 -60.250 0.577
28 -0.06693 0.03099 1.00000 -60.250 -60.000 0.578
29 -0.06743 0.03246 1.00000 -60.000 -59.750 0.579
30 -0.06793 0.03392 1.00000 -59.750 -59.500 0.592
31 -0.06844 0.03539 1.00000 -59.500 -59.250 0.588
32 -0.06894 0.03686 1.00000 -59.250 -59.000 0.596
33 -0.06944 0.03832 1.00000 -59.000 -58.750 0.597
34 -0.06995 0.03979 1.00000 -58.750 -58.500 0.620
35 -0.07045 0.04126 1.00000 -58.500 -58.250 0.612
36 -0.07096 0.04274 1.00000 -58.250 -58.000 0.619
37 -0.07146 0.04421 1.00000 -58.000 -57.750 0.613
38 -0.07197 0.04568 1.00000 -57.750 -57.500 0.625
39 -0.07247 0.04716 1.00000 -57.500 -57.250 0.623
40 -0.07298 0.04863 1.00000 -57.250 -57.000 0.633
41 -0.07349 0.05011 1.00000 -57.000 -56.750 0.629
42 -0.07399 0.05159 1.00000 -56.750 -56.500 0.655
43 -0.07450 0.05307 1.00000 -56.500 -56.250 0.653
44 -0.07501 0.05456 1.00000 -56.250 -56.000 0.655
45 -0.07552 0.05604 1.00000 -56.000 -55.750 0.666
46 -0.07603 0.05753 1.00000 -55.750 -55.500 0.672
47 -0.07654 0.05901 1.00000 -55.500 -55.250 0.677
48 -0.07705 0.06050 1.00000 -55.250 -55.000 0.685
49 -0.07756 0.06200 1.00000 -55.000 -54.750 0.683
50 -0.07807 0.06349 1.00000 -54.750 -54.500 0.693
51 -0.07858 0.06499 1.00000 -54.500 -54.250 0.708
52 -0.07910 0.06648 1.00000 -54.250 -54.000 0.705
53 -0.07961 0.06798 1.00000 -54.000 -53.750 0.716
54 -0.08012 0.06948 1.00000 -53.750 -53.500 0.717
55 -0.08063 0.07098 1.00000 -53.500 -53.250 0.724
56 -0.08115 0.07249 1.00000 -53.250 -53.000 0.739
57 -0.08166 0.07400 1.00000 -53.000 -52.750 0.735
58 -0.08220 0.07551 1.00000 -52.750 -52.500 0.760
59 -0.08269 0.07701 1.00000 -52.500 -52.250 0.752
60 -0.08321 0.07854 1.00000 -52.250 -52.000 0.766
61 -0.08373 0.08005 1.00000 -52.000 -51.750 0.765
62 -0.08425 0.08157 1.00000 -51.750 -51.500 0.779
63 -0.08475 0.08310 1.00000 -51.500 -51.250 0.778
64 -0.08526 0.08463 1.00000 -51.250 -51.000 0.779
65 -0.08578 0.08616 1.00000 -51.000 -50.750 0.784
66 -0.08632 0.08769 1.00000 -50.750 -50.500 0.800
67 -0.08684 0.08924 1.00000 -50.500 -50.250 0.789
68 -0.08737 0.09076 1.00000 -50.250 -50.000 0.786
69 -0.08791 0.09231 1.00000 -50.000 -49.750 0.793
70 -0.08846 0.09386 1.00000 -49.750 -49.500 0.795
71 -0.08898 0.09540 1.00000 -49.500 -49.250 0.791
72 -0.08953 0.09696 1.00000 -49.250 -49.000 0.812
73 -0.09007 0.09851 1.00000 -49.000 -48.750 0.802
74 -0.09060 0.10007 1.00000 -48.750 -48.500 0.808
75 -0.09115 0.10164 1.00000 -48.500 -48.250 0.813
76 -0.09169 0.10321 1.00000 -48.250 -48.000 0.823
77 -0.09223 0.10477 1.00000 -48.000 -47.750 0.827
78 -0.09277 0.10635 1.00000 -47.750 -47.500 0.835
79 -0.09332 0.10793 1.00000 -47.500 -47.250 0.836
80 -0.09384 0.10952 1.00000 -47.250 -47.000 0.842
81 -0.09439 0.11111 1.00000 -47.000 -46.750 0.841
82 -0.09493 0.11270 1.00000 -46.750 -46.500 0.848
83 -0.09549 0.11430 1.00000 -46.500 -46.250 0.848
84 -0.09604 0.11590 1.00000 -46.250 -46.000 0.855
85 -0.09659 0.11751 1.00000 -46.000 -45.750 0.856
86 -0.09714 0.11912 1.00000 -45.750 -45.500 0.864
87 -0.09760 0.12071 1.00000 -45.500 -45.250 0.864
88 -0.09812 0.12231 1.00000 -45.250 -45.000 0.863
89 -0.09867 0.12393 1.00000 -45.000 -44.750 0.867
90 -0.09924 0.12556 1.00000 -44.750 -44.500 0.871
91 -0.09980 0.12720 1.00000 -44.500 -44.250 0.872
92 -0.10035 0.12883 1.00000 -44.250 -44.000 0.865
93 -0.10092 0.13048 1.00000 -44.000 -43.750 0.872
94 -0.10148 0.13213 1.00000 -43.750 -43.500 0.872
95 -0.10205 0.13379 1.00000 -43.500 -43.250 0.870
96 -0.10262 0.13545 1.00000 -43.250 -43.000 0.873
97 -0.10319 0.13712 1.00000 -43.000 -42.750 0.874
98 -0.10376 0.13878 1.00000 -42.750 -42.500 0.879
99 -0.10433 0.14045 1.00000 -42.500 -42.250 0.888
100 -0.10489 0.14213 1.00000 -42.250 -42.000 0.883
101 -0.10547 0.14381 1.00000 -42.000 -41.750 0.883
102 -0.10605 0.14551 1.00000 -41.750 -41.500 0.887
103 -0.10664 0.14720 1.00000 -41.500 -41.250 0.888
104 -0.10721 0.14890 1.00000 -41.250 -41.000 0.894
105 -0.10781 0.15061 1.00000 -41.000 -40.750 0.895
106 -0.10834 0.15233 1.00000 -40.750 -40.500 0.896
107 -0.10893 0.15405 1.00000 -40.500 -40.250 0.898
108 -0.10953 0.15577 1.00000 -40.250 -40.000 0.891
109 -0.11011 0.15751 1.00000 -40.000 -39.750 0.896
110 -0.11069 0.15926 1.00000 -39.750 -39.500 0.890
111 -0.11129 0.16101 1.00000 -39.500 -39.250 0.891
112 -0.11189 0.16277 1.00000 -39.250 -39.000 0.887
113 -0.11249 0.16453 1.00000 -39.000 -38.750 0.888
114 -0.11310 0.16630 1.00000 -38.750 -38.500 0.874
115 -0.11370 0.16808 1.00000 -38.500 -38.250 0.879
116 -0.11431 0.16987 1.00000 -38.250 -38.000 0.867
117 -0.11492 0.17165 1.00000 -38.000 -37.750 0.869
118 -0.11553 0.17343 1.00000 -37.750 -37.500 0.861
119 -0.11615 0.17524 1.00000 -37.500 -37.250 0.863
120 -0.11677 0.17705 1.00000 -37.250 -37.000 0.856
121 -0.11738 0.17888 1.00000 -37.000 -36.750 0.858
122 -0.11801 0.18071 1.00000 -36.750 -36.500 0.861
123 -0.11863 0.18254 1.00000 -36.500 -36.250 0.864
124 -0.11926 0.18437 1.00000 -36.250 -36.000 0.860
125 -0.11989 0.18623 1.00000 -36.000 -35.750 0.862
126 -0.12051 0.18809 1.00000 -35.750 -35.500 0.858
127 -0.12115 0.18996 1.00000 -35.500 -35.250 0.861
128 -0.12179 0.19185 1.00000 -35.250 -35.000 0.853
129 -0.12244 0.19374 1.00000 -35.000 -34.750 0.860
130 -0.12309 0.19566 1.00000 -34.750 -34.500 0.858
131 -0.12371 0.19756 1.00000 -34.500 -34.250 0.854
132 -0.12437 0.19946 1.00000 -34.250 -34.000 0.851
133 -0.12503 0.20139 1.00000 -34.000 -33.750 0.857
134 -0.12572 0.20333 1.00000 -33.750 -33.500 0.864
135 -0.12638 0.20526 1.00000 -33.500 -33.250 0.865
136 -0.12709 0.20721 1.00000 -33.250 -33.000 0.831
137 -0.12775 0.20917 1.00000 -33.000 -32.750 0.829
138 -0.12842 0.21114 1.00000 -32.750 -32.500 0.852
139 -0.12910 0.21313 1.00000 -32.500 -32.250 0.853
140 -0.12977 0.21512 1.00000 -32.250 -32.000 0.878
141 -0.13045 0.21713 1.00000 -32.000 -31.750 0.884
142 -0.13114 0.21914 1.00000 -31.750 -31.500 0.908
143 -0.13182 0.22117 1.00000 -31.500 -31.250 0.908
144 -0.13251 0.22321 1.00000 -31.250 -31.000 0.929
145 -0.13321 0.22526 1.00000 -31.000 -30.750 0.931
146 -0.13391 0.22732 1.00000 -30.750 -30.500 0.952
147 -0.13461 0.22939 1.00000 -30.500 -30.250 0.954
148 -0.13532 0.23147 1.00000 -30.250 -30.000 0.972
149 -0.13603 0.23357 1.00000 -30.000 -29.750 0.973
150 -0.13674 0.23567 1.00000 -29.750 -29.500 0.980
151 -0.13746 0.23779 1.00000 -29.500 -29.250 0.982
152 -0.13818 0.23993 1.00000 -29.250 -29.000 0.990
153 -0.13891 0.24207 1.00000 -29.000 -28.750 0.994
154 -0.13964 0.24423 1.00000 -28.750 -28.500 0.995
155 -0.14038 0.24640 1.00000 -28.500 -28.250 0.999
156 -0.14112 0.24859 1.00000 -28.250 -28.000 0.992
157 -0.14186 0.25079 1.00000 -28.000 -27.750 1.001
158 -0.14261 0.25300 1.00000 -27.750 -27.500 1.004
159 -0.14336 0.25522 1.00000 -27.500 -27.250 1.006
160 -0.14412 0.25746 1.00000 -27.250 -27.000 1.007
161 -0.14489 0.25972 1.00000 -27.000 -26.750 1.012
162 -0.14565 0.26199 1.00000 -26.750 -26.500 1.005
163 -0.14643 0.26427 1.00000 -26.500 -26.250 1.009
164 -0.14721 0.26657 1.00000 -26.250 -26.000 1.016
165 -0.14799 0.26889 1.00000 -26.000 -25.750 1.020
166 -0.14878 0.27122 1.00000 -25.750 -25.500 1.028
167 -0.14957 0.27356 1.00000 -25.500 -25.250 1.033
168 -0.15037 0.27592 1.00000 -25.250 -25.000 1.040
169 -0.15118 0.27830 1.00000 -25.000 -24.750 1.041
170 -0.15199 0.28070 1.00000 -24.750 -24.500 1.047
171 -0.15280 0.28311 1.00000 -24.500 -24.250 1.053
172 -0.15363 0.28554 1.00000 -24.250 -24.000 1.052
173 -0.15445 0.28798 1.00000 -24.000 -23.750 1.056
174 -0.15529 0.29045 1.00000 -23.750 -23.500 1.054
175 -0.15613 0.29293 1.00000 -23.500 -23.250 1.056
176 -0.15697 0.29543 1.00000 -23.250 -23.000 1.063
177 -0.15783 0.29795 1.00000 -23.000 -22.750 1.074
178 -0.15869 0.30049 1.00000 -22.750 -22.500 1.061
179 -0.15955 0.30304 1.00000 -22.500 -22.250 1.061
180 -0.16042 0.30562 1.00000 -22.250 -22.000 1.063
181 -0.16130 0.30822 1.00000 -22.000 -21.750 1.065
182 -0.16219 0.31083 1.00000 -21.750 -21.500 1.054
183 -0.16308 0.31347 1.00000 -21.500 -21.250 1.069
184 -0.16398 0.31613 1.00000 -21.250 -21.000 1.064
185 -0.16488 0.31881 1.00000 -21.000 -20.750 1.057
186 -0.16580 0.32151 1.00000 -20.750 -20.500 1.054
187 -0.16672 0.32423 1.00000 -20.500 -20.250 1.057
188 -0.16764 0.32697 1.00000 -20.250 -20.000 1.047
189 -0.16858 0.32974 1.00000 -20.000 -19.750 1.048
190 -0.16952 0.33253 1.00000 -19.750 -19.500 1.067
191 -0.17048 0.33535 1.00000 -19.500 -19.250 1.061
192 -0.17144 0.33818 1.00000 -19.250 -19.000 1.072
193 -0.17240 0.34104 1.00000 -19.000 -18.750 1.084
194 -0.17338 0.34393 1.00000 -18.750 -18.500 1.115
195 -0.17436 0.34684 1.00000 -18.500 -18.250 1.108
196 -0.17536 0.34978 1.00000 -18.250 -18.000 1.128
197 -0.17636 0.35274 1.00000 -18.000 -17.750 1.129
198 -0.17737 0.35573 1.00000 -17.750 -17.500 1.145
199 -0.17839 0.35875 1.00000 -17.500 -17.250 1.149
200 -0.17942 0.36179 1.00000 -17.250 -17.000 1.163
201 -0.18046 0.36487 1.00000 -17.000 -16.750 1.160
202 -0.18151 0.36797 1.00000 -16.750 -16.500 1.179
203 -0.18256 0.37110 1.00000 -16.500 -16.250 1.177
204 -0.18363 0.37426 1.00000 -16.250 -16.000 1.183
205 -0.18471 0.37744 1.00000 -16.000 -15.750 1.187
206 -0.18580 0.38066 1.00000 -15.750 -15.500 1.196
207 -0.18690 0.38391 1.00000 -15.500 -15.250 1.206
208 -0.18800 0.38720 1.00000 -15.250 -15.000 1.219
209 -0.18912 0.39051 1.00000 -15.000 -14.750 1.212
210 -0.19026 0.39386 1.00000 -14.750 -14.500 1.220
211 -0.19140 0.39724 1.00000 -14.500 -14.250 1.208
212 -0.19255 0.40066 1.00000 -14.250 -14.000 1.226
213 -0.19372 0.40411 1.00000 -14.000 -13.750 1.230
214 -0.19490 0.40759 1.00000 -13.750 -13.500 1.245
215 -0.19609 0.41111 1.00000 -13.500 -13.250 1.220
216 -0.19729 0.41467 1.00000 -13.250 -13.000 1.262
217 -0.19850 0.41827 1.00000 -13.000 -12.750 1.255
218 -0.19973 0.42190 1.00000 -12.750 -12.500 1.244
219 -0.20097 0.42558 1.00000 -12.500 -12.250 1.264
220 -0.20223 0.42929 1.00000 -12.250 -12.000 1.256
221 -0.20350 0.43305 1.00000 -12.000 -11.750 1.261
222 -0.20478 0.43684 1.00000 -11.750 -11.500 1.255
223 -0.20608 0.44068 1.00000 -11.500 -11.250 1.246
224 -0.20739 0.44456 1.00000 -11.250 -11.000 1.248
225 -0.20871 0.44849 1.00000 -11.000 -10.750 1.257
226 -0.21006 0.45246 1.00000 -10.750 -10.500 1.238
227 -0.21141 0.45648 1.00000 -10.500 -10.250 1.236
228 -0.21278 0.46054 1.00000 -10.250 -10.000 1.232
229 -0.21417 0.46465 1.00000 -10.000 -9.750 1.232
230 -0.21558 0.46881 1.00000 -9.750 -9.500 1.230
231 -0.21700 0.47302 1.00000 -9.500 -9.250 1.233
232 -0.21844 0.47728 1.00000 -9.250 -9.000 1.242
233 -0.21990 0.48160 1.00000 -9.000 -8.750 1.232
234 -0.22137 0.48596 1.00000 -8.750 -8.500 1.248
235 -0.22287 0.49038 1.00000 -8.500 -8.250 1.244
236 -0.22438 0.49486 1.00000 -8.250 -8.000 1.260
237 -0.22591 0.49939 1.00000 -8.000 -7.750 1.252
238 -0.22746 0.50399 1.00000 -7.750 -7.500 1.271
239 -0.22903 0.50864 1.00000 -7.500 -7.250 1.265
240 -0.23062 0.51335 1.00000 -7.250 -7.000 1.277
241 -0.23223 0.51812 1.00000 -7.000 -6.750 1.256
242 -0.23387 0.52296 1.00000 -6.750 -6.500 1.286
243 -0.23550 0.52786 1.00000 -6.500 -6.250 1.292
244 -0.23717 0.53282 1.00000 -6.250 -6.000 1.277
245 -0.23884 0.53784 1.00000 -6.000 -5.750 1.297
246 -0.24055 0.54294 1.00000 -5.750 -5.500 1.298
247 -0.24229 0.54810 1.00000 -5.500 -5.250 1.269
248 -0.24404 0.55336 1.00000 -5.250 -5.000 1.261
249 -0.24585 0.55869 1.00000 -5.000 -4.750 1.271
250 -0.24768 0.56407 1.00000 -4.750 -4.500 1.280
251 -0.24954 0.56957 1.00000 -4.500 -4.250 1.296
252 -0.25142 0.57514 1.00000 -4.250 -4.000 1.268
253 -0.25332 0.58079 1.00000 -4.000 -3.750 1.291
254 -0.25527 0.58653 1.00000 -3.750 -3.500 1.271
255 -0.25723 0.59236 1.00000 -3.500 -3.250 1.280
256 -0.25922 0.59827 1.00000 -3.250 -3.000 1.290
257 -0.26124 0.60425 1.00000 -3.000 -2.750 1.300
258 -0.26333 0.61037 1.00000 -2.750 -2.500 1.326
259 -0.26542 0.61656 1.00000 -2.500 -2.250 1.303
260 -0.26756 0.62285 1.00000 -2.250 -2.000 1.332
261 -0.26972 0.62924 1.00000 -2.000 -1.750 1.329
262 -0.27190 0.63571 1.00000 -1.750 -1.500 1.350
263 -0.27412 0.64230 1.00000 -1.500 -1.250 1.372
264 -0.27634 0.64903 1.00000 -1.250 -1.000 1.345
265 -0.27863 0.65584 1.00000 -1.000 -0.750 1.369
266 -0.28098 0.66277 1.00000 -0.750 -0.500 1.367
267 -0.28336 0.66979 1.00000 -0.500 -0.250 1.388
268 -0.28576 0.67694 1.00000 -0.250 0.000 1.369
269 -0.28823 0.68425 1.00000 0.000 0.250 1.375
270 -0.29071 0.69169 1.00000 0.250 0.500 1.372
271 -0.29325 0.69924 1.00000 0.500 0.750 1.369
272 -0.29585 0.70689 1.00000 0.750 1.000 1.356
273 -0.29853 0.71474 1.00000 1.000 1.250 1.368
274 -0.30125 0.72272 1.00000 1.250 1.500 1.360
275 -0.30400 0.73086 1.00000 1.500 1.750 1.361
276 -0.30679 0.73912 1.00000 1.750 2.000 1.354
277 -0.30967 0.74757 1.00000 2.000 2.250 1.368
278 -0.31258 0.75620 1.00000 2.250 2.500 1.334
279 -0.31554 0.76498 1.00000 2.500 2.750 1.356
280 -0.31861 0.77395 1.00000 2.750 3.000 1.333
281 -0.32173 0.78312 1.00000 3.000 3.250 1.338
282 -0.32486 0.79244 1.00000 3.250 3.500 1.314
283 -0.32811 0.80197 1.00000 3.500 3.750 1.333
284 -0.33139 0.81169 1.00000 3.750 4.000 1.327
285 -0.33471 0.82155 1.00000 4.000 4.250 1.327
286 -0.33813 0.83170 1.00000 4.250 4.500 1.329
287 -0.34164 0.84204 1.00000 4.500 4.750 1.329
288 -0.34521 0.85262 1.00000 4.750 5.000 1.317
289 -0.34882 0.86348 1.00000 5.000 5.250 1.307
290 -0.35258 0.87460 1.00000 5.250 5.500 1.311
291 -0.35638 0.88595 1.00000 5.500 5.750 1.311
292 -0.36030 0.89752 1.00000 5.750 6.000 1.295
293 -0.36433 0.90936 1.00000 6.000 6.250 1.277
294 -0.36841 0.92149 1.00000 6.250 6.500 1.292
295 -0.37266 0.93395 1.00000 6.500 6.750 1.304
296 -0.37693 0.94663 1.00000 6.750 7.000 1.277
297 -0.38135 0.95970 1.00000 7.000 7.250 1.282
298 -0.38588 0.97306 1.00000 7.250 7.500 1.300
299 -0.39048 0.98677 1.00000 7.500 7.750 1.292
300 -0.39481 1.00000 0.99917 7.750 8.000 1.320
301 -0.39402 1.00000 0.98501 8.000 8.250 1.300
302 -0.39322 1.00000 0.97088 8.250 8.500 1.321
303 -0.39239 1.00000 0.95680 8.500 8.750 1.310
304 -0.39159 1.00000 0.94272 8.750 9.000 1.299
305 -0.39078 1.00000 0.92866 9.000 9.250 1.303
306 -0.38999 1.00000 0.91467 9.250 9.500 1.299
307 -0.38917 1.00000 0.90081 9.500 9.750 1.295
308 -0.38838 1.00000 0.88688 9.750 10.000 1.258
309 -0.38758 1.00000 0.87296 10.000 10.250 1.294
310 -0.38677 1.00000 0.85906 10.250 10.500 1.253
311 -0.38601 1.00000 0.84522 10.500 10.750 1.254
312 -0.38519 1.00000 0.83137 10.750 11.000 1.206
313 -0.38439 1.00000 0.81753 11.000 11.250 1.194
314 -0.38362 1.00000 0.80379 11.250 11.500 1.207
315 -0.38283 1.00000 0.79010 11.500 11.750 1.214
316 -0.38205 1.00000 0.77637 11.750 12.000 1.231
317 -0.38124 1.00000 0.76265 12.000 12.250 1.204
318 -0.38048 1.00000 0.74900 12.250 12.500 1.202
319 -0.37972 1.00000 0.73535 12.500 12.750 1.208
320 -0.37896 1.00000 0.72174 12.750 13.000 1.244
321 -0.37817 1.00000 0.70820 13.000 13.250 1.234
322 -0.37740 1.00000 0.69464 13.250 13.500 1.230
323 -0.37659 1.00000 0.68107 13.500 13.750 1.212
324 -0.37582 1.00000 0.66758 13.750 14.000 1.239
325 -0.37502 1.00000 0.65412 14.000 14.250 1.237
326 -0.37423 1.00000 0.64066 14.250 14.500 1.228
327 -0.37348 1.00000 0.62715 14.500 14.750 1.229
328 -0.37273 1.00000 0.61372 14.750 15.000 1.243
329 -0.37197 1.00000 0.60026 15.000 15.250 1.245
330 -0.37122 1.00000 0.58689 15.250 15.500 1.238
331 -0.37047 1.00000 0.57351 15.500 15.750 1.255
332 -0.36971 1.00000 0.56015 15.750 16.000 1.248
333 -0.36896 1.00000 0.54682 16.000 16.250 1.259
334 -0.36820 1.00000 0.53350 16.250 16.500 1.261
335 -0.36744 1.00000 0.52021 16.500 16.750 1.251
336 -0.36672 1.00000 0.50693 16.750 17.000 1.268
337 -0.36599 1.00000 0.49367 17.000 17.250 1.267
338 -0.36522 1.00000 0.48050 17.250 17.500 1.268
339 -0.36443 1.00000 0.46726 17.500 17.750 1.270
340 -0.36369 1.00000 0.45404 17.750 18.000 1.279
341 -0.36295 1.00000 0.44081 18.000 18.250 1.260
342 -0.36216 1.00000 0.42749 18.250 18.500 1.272
343 -0.36140 1.00000 0.41432 18.500 18.750 1.267
344 -0.36067 1.00000 0.40114 18.750 19.000 1.276
345 -0.35995 1.00000 0.38796 19.000 19.250 1.281
346 -0.35917 1.00000 0.37477 19.250 19.500 1.279
347 -0.35843 1.00000 0.36162 19.500 19.750 1.303
348 -0.35770 1.00000 0.34853 19.750 20.000 1.283
349 -0.35697 1.00000 0.33540 20.000 20.250 1.288
350 -0.35624 1.00000 0.32228 20.250 20.500 1.279
351 -0.35549 1.00000 0.30913 20.500 20.750 1.280
352 -0.35472 1.00000 0.29609 20.750 21.000 1.284
353 -0.35394 1.00000 0.28305 21.000 21.250 1.273
354 -0.35323 1.00000 0.27000 21.250 21.500 1.283
355 -0.35249 1.00000 0.25688 21.500 21.750 1.282
356 -0.35173 1.00000 0.24382 21.750 22.000 1.270
357 -0.35102 1.00000 0.23077 22.000 22.250 1.266
358 -0.35028 1.00000 0.21771 22.250 22.500 1.276
359 -0.34953 1.00000 0.20468 22.500 22.750 1.261
360 -0.34879 1.00000 0.19168 22.750 23.000 1.269
361 -0.34805 1.00000 0.17860 23.000 23.250 1.243
362 -0.34731 1.00000 0.16556 23.250 23.500 1.255
363 -0.34658 1.00000 0.15258 23.500 23.750 1.247
364 -0.34584 1.00000 0.13956 23.750 24.000 1.258
365 -0.34506 1.00000 0.12654 24.000 24.250 1.233
366 -0.34435 1.00000 0.11354 24.250 24.500 1.219
367 -0.34363 1.00000 0.10050 24.500 24.750 1.231
368 -0.34291 1.00000 0.08745 24.750 25.000 1.220
369 -0.34216 1.00000 0.07438 25.000 25.250 1.213
370 -0.34141 1.00000 0.06131 25.250 25.500 1.195
371 -0.34064 1.00000 0.04832 25.500 25.750 1.211
372 -0.33989 1.00000 0.03530 25.750 26.000 1.209
373 -0.33910 1.00000 0.02227 26.000 26.250 1.198
374 -0.33837 1.00000 0.00914 26.250 26.500 1.186
375 -0.33762 1.00000 -0.00393 26.500 26.750 1.199
376 -0.33683 1.00000 -0.01701 26.750 27.000 1.201
377 -0.33609 1.00000 -0.03011 27.000 27.250 1.196
378 -0.33537 1.00000 -0.04318 27.250 27.500 1.157
379 -0.33466 1.00000 -0.05628 27.500 27.750 1.169
380 -0.33392 1.00000 -0.06933 27.750 28.000 1.208
381 -0.33319 1.00000 -0.08245 28.000 28.250 1.202
382 -0.33249 1.00000 -0.09553 28.250 28.500 1.218
383 -0.33175 1.00000 -0.10863 28.500 28.750 1.208
384 -0.33103 1.00000 -0.12175 28.750 29.000 1.236
385 -0.33027 1.00000 -0.13490 29.000 29.250 1.221
386 -0.32950 1.00000 -0.14799 29.250 29.500 1.225
387 -0.32872 1.00000 -0.16118 29.500 29.750 1.219
388 -0.32799 1.00000 -0.17433 29.750 30.000 1.223
389 -0.32725 1.00000 -0.18754 30.000 30.250 1.224
390 -0.32651 1.00000 -0.20076 30.250 30.500 1.219
391 -0.32577 1.00000 -0.21394 30.500 30.750 1.214
392 -0.32502 1.00000 -0.22713 30.750 31.000 1.229
393 -0.32428 1.00000 -0.24034 31.000 31.250 1.233
394 -0.32351 1.00000 -0.25352 31.250 31.500 1.246
395 -0.32277 1.00000 -0.26673 31.500 31.750 1.245
396 -0.32196 1.00000 -0.27986 31.750 32.000 1.267
397 -0.32122 1.00000 -0.29311 32.000 32.250 1.261
398 -0.32042 1.00000 -0.30647 32.250 32.500 1.261
399 -0.31965 1.00000 -0.31976 32.500 32.750 1.274
400 -0.31887 1.00000 -0.33299 32.750 33.000 1.257
401 -0.31812 1.00000 -0.34633 33.000 33.250 1.267
402 -0.31735 1.00000 -0.35968 33.250 33.500 1.252
403 -0.31661 1.00000 -0.37309 33.500 33.750 1.262
404 -0.31586 1.00000 -0.38648 33.750 34.000 1.251
405 -0.31509 1.00000 -0.39987 34.000 34.250 1.235
406 -0.31431 1.00000 -0.41339 34.250 34.500 1.245
407 -0.31355 1.00000 -0.42683 34.500 34.750 1.242
408 -0.31279 1.00000 -0.44035 34.750 35.000 1.218
409 -0.31203 1.00000 -0.45387 35.000 35.250 1.213
410 -0.31126 1.00000 -0.46741 35.250 35.500 1.213
411 -0.31051 1.00000 -0.48098 35.500 35.750 1.188
412 -0.30975 1.00000 -0.49461 35.750 36.000 1.201
413 -0.30897 1.00000 -0.50819 36.000 36.250 1.194
414 -0.30817 1.00000 -0.52182 36.250 36.500 1.166
415 -0.30740 1.00000 -0.53541 36.500 36.750 1.167
416 -0.30659 1.00000 -0.54907 36.750 37.000 1.185
417 -0.30577 1.00000 -0.56275 37.000 37.250 1.171
418 -0.30496 1.00000 -0.57644 37.250 37.500 1.160
419 -0.30413 1.00000 -0.59016 37.500 37.750 1.154
420 -0.30336 1.00000 -0.60392 37.750 38.000 1.153
421 -0.30255 1.00000 -0.61773 38.000 38.250 1.165
422 -0.30179 1.00000 -0.63160 38.250 38.500 1.159
423 -0.30102 1.00000 -0.64544 38.500 38.750 1.139
424 -0.30022 1.00000 -0.65936 38.750 39.000 1.133
425 -0.29946 1.00000 -0.67328 39.000 39.250 1.162
426 -0.29867 1.00000 -0.68725 39.250 39.500 1.135
427 -0.29789 1.00000 -0.70124 39.500 39.750 1.156
428 -0.29708 1.00000 -0.71525 39.750 40.000 1.142
429 -0.29624 1.00000 -0.72925 40.000 40.250 1.147
430 -0.29541 1.00000 -0.74334 40.250 40.500 1.148
431 -0.29458 1.00000 -0.75732 40.500 40.750 1.150
432 -0.29378 1.00000 -0.77148 40.750 41.000 1.151
433 -0.29299 1.00000 -0.78567 41.000 41.250 1.146
434 -0.29221 1.00000 -0.79991 41.250 41.500 1.150
435 -0.29142 1.00000 -0.81418 41.500 41.750 1.154
436 -0.29063 1.00000 -0.82848 41.750 42.000 1.162
437 -0.28983 1.00000 -0.84283 42.000 42.250 1.164
438 -0.28904 1.00000 -0.85722 42.250 42.500 1.153
439 -0.28824 1.00000 -0.87165 42.500 42.750 1.154
440 -0.28744 1.00000 -0.88612 42.750 43.000 1.130
441 -0.28664 1.00000 -0.90063 43.000 43.250 1.140
442 -0.28583 1.00000 -0.91518 43.250 43.500 1.109
443 -0.28503 1.00000 -0.92978 43.500 43.750 1.113
444 -0.28422 1.00000 -0.94442 43.750 44.000 1.110
445 -0.28340 1.00000 -0.95910 44.000 44.250 1.106
446 -0.28259 1.00000 -0.97383 44.250 44.500 1.102
447 -0.28177 1.00000 -0.98861 44.500 44.750 1.100
448 -0.27999 0.99657 -1.00000 44.750 45.000 1.090
449 -0.27509 0.98202 -1.00000 45.000 45.250 1.103
450 -0.27032 0.96784 -1.00000 45.250 45.500 1.115
451 -0.26567 0.95401 -1.00000 45.500 45.750 1.101
452 -0.26114 0.94053 -1.00000 45.750 46.000 1.098
453 -0.25671 0.92739 -1.00000 46.000 46.250 1.097
454 -0.25240 0.91456 -1.00000 46.250 46.500 1.075
455 -0.24818 0.90204 -1.00000 46.500 46.750 1.088
456 -0.24407 0.88981 -1.00000 46.750 47.000 1.068
457 -0.24005 0.87787 -1.00000 47.000 47.250 1.050
458 -0.23613 0.86620 -1.00000 47.250 47.500 1.053
459 -0.23229 0.85480 -1.00000 47.500 47.750 1.043
460 -0.22854 0.84365 -1.00000 47.750 48.000 1.017
461 -0.22487 0.83275 -1.00000 48.000 48.250 1.034
462 -0.22129 0.82209 -1.00000 48.250 48.500 1.011
463 -0.21778 0.81166 -1.00000 48.500 48.750 1.005
464 -0.21434 0.80145 -1.00000 48.750 49.000 0.995
465 -0.21098 0.79145 -1.00000 49.000 49.250 1.002
466 -0.20769 0.78167 -1.00000 49.250 49.500 0.984
467 -0.20446 0.77208 -1.00000 49.500 49.750 0.991
468 -0.20130 0.76269 -1.00000 49.750 50.000 0.978
469 -0.19820 0.75348 -1.00000 50.000 50.250 0.982
470 -0.19517 0.74446 -1.00000 50.250 50.500 0.966
471 -0.19219 0.73562 -1.00000 50.500 50.750 0.966
472 -0.18928 0.72694 -1.00000 50.750 51.000 0.958
473 -0.18641 0.71844 -1.00000 51.000 51.250 0.963
474 -0.18360 0.71009 -1.00000 51.250 51.500 0.953
475 -0.18085 0.70190 -1.00000 51.500 51.750 0.953
476 -0.17814 0.69386 -1.00000 51.750 52.000 0.946
477 -0.17549 0.68597 -1.00000 52.000 52.250 0.951
478 -0.17288 0.67822 -1.00000 52.250 52.500 0.944
479 -0.17032 0.67061 -1.00000 52.500 52.750 0.945
480 -0.16781 0.66313 -1.00000 52.750 53.000 1.000
481 -0.16533 0.65578 -1.00000 53.000 53.250 1.000
482 -0.16290 0.64856 -1.00000 53.250 53.500 1.000
483 -0.16052 0.64147 -1.00000 53.500 53.750 1.000
484 -0.15817 0.63449 -1.00000 53.750 54.000 1.000


_diffrn.ambient_temperature      298
_diffrn.ambient_environment      vacuum
_exptl_crystal.colour            'dark brown'
_exptl_crystal.description       irregular
_diffrn_radiation_wavelength.value 0.0251
_diffrn_source.device            'electron gun'
_diffrn_source.make              'JEOL JSM-2300ED, LaB6'
_diffrn_source.voltage           200
_diffrn_radiation.probe          electron
_diffrn_radiation.monochromator  none
_diffrn_detector.description     'hybrid pixel array detector'
_diffrn_detector.make            'Rigaku HyPix-ED'
_diffrn_measurement.device_class 'electron diffractometer'
_diffrn_measurement.device_make  'Rigaku XtaLAB Synergy-ED'
_diffrn_measurement.method       'continuous rotation electron diffraction'
_diffrn_measurement.specimen_support 
;
continuous carbon film on copper grid, 200 mesh
;
_exptl.special_details           
;
Gatan Elsa cryo-transfer holder model 698. Temperature controller model 1905
;
_exptl_crystal.preparation       'dry powder deposited on grid'
_exptl.crystals_number           1
_diffrn_source.ed_diffracting_area_selection SAED
_diffrn_measurement.rotation_mode rotation
_refine.diffraction_theory       kinematical
_refine.diffraction_theory_details ?
_diffrn_measurement.sample_tracking no
_diffrn_measurement.sample_tracking_method .
_computing.sample_tracking       .
_diffrn_radiation.illumination_mode parallel
_diffrn_source.size              
;
SAED nominal aperture diameter 100 um, corresponding to a diameter of about 2 um
at the image plane.
;
_diffrn_measurement.method_precession no
_diffrn.precession_semi_angle    .
_refine_diff.potential_max       ?
_refine_diff.potential_min       ?
_refine_diff.potential_RMS       ?
_exptl_crystal.mosaicity         ?
_exptl_crystal.mosaic_method     ?
_exptl_crystal.mosaic_block_size ?
_diffrn_source.convergence_angle ?
_refine_ls.sample_thickness      .
_refine_ls.sample_shape_expression .
_refine_ls.sample_shape_details  .
_diffrn.flux_density             ?
_diffrn.total_dose               ?
_diffrn.total_exposure_time      2
