# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_xb0470_0m
_audit_block_doi                 10.5517/ccdc.csd.cc257ppt
_database_code_depnum_ccdc_archive 'CCDC 2003396'
loop_
_audit_author_name
_audit_author_address
'Bin Liu'
;Northwest University
China
;
_audit_update_record             
;
2024-01-06 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_xb0470_0m           
;
PROBLEM: Short Inter D-H..H-D H4 ..H4 . 1.71 Ang. 
RESPONSE: constraint hydrogen_treatment resulted in the Alert problem
;
# end Validation Reply Form
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H24 N4 O10 Ru2, 4(H2 O), 2(H2 O)'
_chemical_formula_sum            'C10 H32 N4 O16 Ru2'
_chemical_formula_weight         666.53

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.2244(16)
_cell_length_b                   13.610(3)
_cell_length_c                   11.705(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.217(4)
_cell_angle_gamma                90
_cell_volume                     1147.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    967
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      22.42

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_F_000             672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.396
_shelx_estimated_absorpt_T_min   0.829
_shelx_estimated_absorpt_T_max   0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5689
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.298
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_full        25.098
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2032
_reflns_number_gt                1558
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0295P)²+0.1188P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2032
_refine_ls_number_parameters     170
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0712
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.989
_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
Ru1 Ru 0.11878(5) 0.03411(3) 0.94652(3) 0.02062(13) Uani 1 1 d . . . . .
O1 O 0.1180(4) -0.0863(2) 1.0332(2) 0.0250(7) Uani 1 1 d . . . . .
O2 O -0.2197(4) -0.1061(2) 0.9098(2) 0.0280(7) Uani 1 1 d . . . . .
O3 O 0.0105(4) -0.0434(2) 0.8072(2) 0.0273(7) Uani 1 1 d . . . . .
O4 O -0.2035(5) -0.1422(2) 0.7283(3) 0.0376(9) Uani 1 1 d . . . . .
O5 O 0.3726(4) -0.0024(2) 0.9040(3) 0.0286(7) Uani 1 1 d . . . . .
H5E H 0.448905 0.041222 0.929708 0.034 Uiso 1 1 d R U . . .
O6 O 0.5770(6) 0.1764(4) 0.8374(6) 0.0957(18) Uani 1 1 d D . . . .
O7 O 0.1788(9) 0.0373(5) 0.4735(5) 0.1010(19) Uani 1 1 d D . . . .
O8 O 0.5177(12) 0.0823(7) 0.6066(9) 0.119(4) Uani 0.805(18) 1 d D . . . .
N1 N 0.1668(5) 0.1629(2) 0.8474(3) 0.0259(9) Uani 1 1 d . . . . .
H1A H 0.290065 0.164934 0.840816 0.031 Uiso 1 1 d R U . . .
N2 N 0.0809(6) 0.3393(3) 0.7187(4) 0.0393(11) Uani 1 1 d . . . . .
H2C H 0.116653 0.391285 0.678148 0.047 Uiso 1 1 d R U . . .
H2D H -0.042797 0.341345 0.723358 0.047 Uiso 1 1 d R U . . .
C1 C -0.1349(6) -0.0965(3) 0.8149(4) 0.0283(11) Uani 1 1 d . . . . .
C2 C 0.0821(8) 0.1603(4) 0.7290(4) 0.0409(13) Uani 1 1 d . . . . .
H2A H -0.050280 0.156720 0.731169 0.049 Uiso 1 1 d R U . . .
H2B H 0.122840 0.102130 0.691889 0.049 Uiso 1 1 d R U . . .
C3 C 0.1205(8) 0.2569(3) 0.9032(4) 0.0385(13) Uani 1 1 d . . . . .
H3A H 0.182007 0.259440 0.978714 0.046 Uiso 1 1 d R U . . .
H3B H -0.010873 0.258460 0.910844 0.046 Uiso 1 1 d R U . . .
C4 C 0.1304(8) 0.2493(4) 0.6588(4) 0.0433(14) Uani 1 1 d . . . . .
H4A H 0.066122 0.246916 0.584129 0.052 Uiso 1 1 d R U . . .
H4B H 0.261342 0.249446 0.649549 0.052 Uiso 1 1 d R U . . .
C5 C 0.1730(8) 0.3450(4) 0.8348(4) 0.0428(14) Uani 1 1 d . . . . .
H5A H 0.135785 0.404086 0.871474 0.051 Uiso 1 1 d R U . . .
H5B H 0.305175 0.346516 0.830634 0.051 Uiso 1 1 d R U . . .
H1 H 0.668(7) 0.149(5) 0.875(5) 0.10(3) Uiso 1 1 d D . . . .
H2 H 0.600(11) 0.234(3) 0.817(7) 0.14(4) Uiso 1 1 d D . . . .
H3 H 0.166(9) 0.070(4) 0.413(3) 0.09(3) Uiso 1 1 d D . . . .
H4 H 0.089(9) 0.040(7) 0.516(6) 0.17(5) Uiso 1 1 d D . . . .
H5 H 0.56(5) 0.05(2) 0.557(10) 0.8(3) Uiso 1 1 d D . . . .
H6 H 0.550(11) 0.078(6) 0.678(2) 0.10(4) Uiso 1 1 d 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
Ru1 O1 1.883(3) 3_557 ?
Ru1 O1 1.927(3) . ?
Ru1 O5 1.997(3) . ?
Ru1 O2 2.035(3) 3_557 ?
Ru1 O3 2.048(3) . ?
Ru1 N1 2.145(3) . ?
Ru1 Ru1 2.3857(8) 3_557 ?
O2 C1 1.314(5) . ?
O3 C1 1.283(5) . ?
O4 C1 1.259(5) . ?
O5 H5E 0.8500 . ?
O6 H1 0.85(2) . ?
O6 H2 0.84(2) . ?
O7 H3 0.84(2) . ?
O7 H4 0.85(2) . ?
O8 H5 0.85(2) . ?
O8 H6 0.86(2) . ?
N1 C2 1.474(6) . ?
N1 C3 1.485(6) . ?
N1 H1A 0.9000 . ?
N2 C4 1.469(6) . ?
N2 C5 1.470(6) . ?
N2 H2C 0.9000 . ?
N2 H2D 0.9000 . ?
C2 C4 1.518(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C3 C5 1.506(6) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9599 . ?
C5 H5A 0.9599 . ?
C5 H5B 0.9600 . ?

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 102.48(11) 3_557 . ?
O1 Ru1 O5 169.78(12) 3_557 . ?
O1 Ru1 O5 87.58(12) . . ?
O1 Ru1 O2 89.29(12) 3_557 3_557 ?
O1 Ru1 O2 89.37(12) . 3_557 ?
O5 Ru1 O2 92.64(12) . 3_557 ?
O1 Ru1 O3 89.84(12) 3_557 . ?
O1 Ru1 O3 88.01(12) . . ?
O5 Ru1 O3 88.72(12) . . ?
O2 Ru1 O3 177.00(11) 3_557 . ?
O1 Ru1 N1 86.82(13) 3_557 . ?
O1 Ru1 N1 170.61(12) . . ?
O5 Ru1 N1 83.16(13) . . ?
O2 Ru1 N1 89.49(13) 3_557 . ?
O3 Ru1 N1 93.33(13) . . ?
O1 Ru1 Ru1 52.07(9) 3_557 3_557 ?
O1 Ru1 Ru1 50.41(8) . 3_557 ?
O5 Ru1 Ru1 137.96(9) . 3_557 ?
O2 Ru1 Ru1 88.94(8) 3_557 3_557 ?
O3 Ru1 Ru1 88.26(8) . 3_557 ?
N1 Ru1 Ru1 138.88(10) . 3_557 ?
Ru1 O1 Ru1 77.52(10) 3_557 . ?
C1 O2 Ru1 119.3(3) . 3_557 ?
C1 O3 Ru1 120.1(3) . . ?
Ru1 O5 H5E 108.8 . . ?
H1 O6 H2 113(7) . . ?
H3 O7 H4 116(6) . . ?
H5 O8 H6 123(8) . . ?
C2 N1 C3 110.1(4) . . ?
C2 N1 Ru1 114.6(3) . . ?
C3 N1 Ru1 114.5(3) . . ?
C2 N1 H1A 105.4 . . ?
C3 N1 H1A 105.6 . . ?
Ru1 N1 H1A 105.7 . . ?
C4 N2 C5 112.0(4) . . ?
C4 N2 H2C 108.4 . . ?
C5 N2 H2C 108.6 . . ?
C4 N2 H2D 109.4 . . ?
C5 N2 H2D 109.0 . . ?
H2C N2 H2D 109.4 . . ?
O4 C1 O3 119.8(4) . . ?
O4 C1 O2 116.8(4) . . ?
O3 C1 O2 123.4(4) . . ?
N1 C2 C4 113.2(4) . . ?
N1 C2 H2A 108.8 . . ?
C4 C2 H2A 108.9 . . ?
N1 C2 H2B 109.0 . . ?
C4 C2 H2B 108.8 . . ?
H2A C2 H2B 108.0 . . ?
N1 C3 C5 112.2(4) . . ?
N1 C3 H3A 109.4 . . ?
C5 C3 H3A 110.1 . . ?
N1 C3 H3B 108.4 . . ?
C5 C3 H3B 108.7 . . ?
H3A C3 H3B 107.9 . . ?
N2 C4 C2 109.5(4) . . ?
N2 C4 H4A 110.1 . . ?
C2 C4 H4A 110.6 . . ?
N2 C4 H4B 109.2 . . ?
C2 C4 H4B 109.3 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C3 109.6(4) . . ?
N2 C5 H5A 109.6 . . ?
C3 C5 H5A 109.8 . . ?
N2 C5 H5B 109.8 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 108.4 . . ?

_refine_diff_density_max         0.413
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_20210416gl_0m_a
_audit_block_doi                 10.5517/ccdc.csd.cc2hh5z5
_database_code_depnum_ccdc_archive 'CCDC 2308507'
loop_
_audit_author_name
_audit_author_address
'Bin Liu'
;Northwest University
China
;
_audit_update_record             
;
2024-01-06 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_20210416gl_0m_a     
;
PROBLEM: Short Inter D...A Contact O11 ..O11' . 0.73 Ang. 
RESPONSE: disordered lattice water O11 resulted the Alert level A and B problem
;
_vrf_PLAT417_20210416gl_0m_a     
;
PROBLEM: Short Inter D-H..H-D H1C ..H8A . 2.03 Ang 
RESPONSE: constraint hydrogen treatment resulted in the Alert level B problem
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H32 N4 O10 Ru2, 10(H2 O), 2(O1.14)'
_chemical_formula_sum            'C14 H56 N4 O22 Ru2'
_chemical_formula_weight         834.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -0.0760 2.5955 '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'

_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                   7.8283(6)
_cell_length_b                   14.3445(11)
_cell_length_c                   14.3344(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.810(2)
_cell_angle_gamma                90
_cell_volume                     1609.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9689
_cell_measurement_theta_min      3.891
_cell_measurement_theta_max      54.934

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    5.674
_shelx_estimated_absorpt_T_min   0.235
_shelx_estimated_absorpt_T_max   0.428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.152
_exptl_absorpt_correction_T_max  0.313
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.34139
_diffrn_radiation_type           GaK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10852
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.793
_diffrn_reflns_theta_max         54.933
_diffrn_reflns_theta_full        53.594
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3029
_reflns_number_gt                2938
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0351P)²+1.9842P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3029
_refine_ls_number_parameters     225
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0626
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.59785(2) 0.56376(2) 0.50543(2) 0.00872(8) Uani 1 1 d . . . . .
N1 N 0.6725(2) 0.66626(13) 0.60872(12) 0.0114(4) Uani 1 1 d . . . . .
H1B H 0.770286 0.691734 0.588536 0.014 Uiso 1 1 d R U . . .
N2 N 0.6480(2) 0.76845(13) 0.78292(12) 0.0131(4) Uani 1 1 d . . . . .
H2D H 0.688193 0.810806 0.824005 0.016 Uiso 1 1 d R U . . .
H2C H 0.551113 0.743616 0.805105 0.016 Uiso 1 1 d R U . . .
C1 C 0.7372(3) 0.38690(15) 0.57165(14) 0.0122(4) Uani 1 1 d . . . . .
C2 C 0.5508(3) 0.74482(15) 0.61994(15) 0.0131(4) Uani 1 1 d . . . . .
H2A H 0.442578 0.720020 0.638613 0.016 Uiso 1 1 d R U . . .
H2B H 0.534228 0.775220 0.560843 0.016 Uiso 1 1 d R U . . .
C3 C 0.7136(3) 0.62355(15) 0.70062(15) 0.0145(4) Uani 1 1 d . . . . .
H3A H 0.798053 0.575789 0.692460 0.017 Uiso 1 1 d R U . . .
H3B H 0.612424 0.594470 0.724019 0.017 Uiso 1 1 d R U . . .
C4 C 0.6098(3) 0.81660(15) 0.69207(15) 0.0147(4) Uani 1 1 d . . . . .
H4A H 0.712081 0.845988 0.670529 0.018 Uiso 1 1 d R U . . .
C5 C 0.7784(3) 0.69327(15) 0.77241(16) 0.0153(4) Uani 1 1 d . . . . .
H5A H 0.882511 0.720414 0.750517 0.018 Uiso 1 1 d R U . . .
C6 C 0.4748(3) 0.89061(17) 0.70752(17) 0.0235(5) Uani 1 1 d . . . . .
H6A H 0.515641 0.934788 0.752934 0.035 Uiso 1 1 d R U . . .
H6B H 0.450372 0.922188 0.649825 0.035 Uiso 1 1 d R U . . .
H6C H 0.372682 0.861528 0.729684 0.035 Uiso 1 1 d R U . . .
C7 C 0.8119(4) 0.64666(18) 0.86589(17) 0.0256(6) Uani 1 1 d . . . . .
H7A H 0.853415 0.692015 0.909918 0.038 Uiso 1 1 d R U . . .
H7B H 0.707795 0.619865 0.888198 0.038 Uiso 1 1 d R U . . .
H7C H 0.895825 0.598485 0.858618 0.038 Uiso 1 1 d R U . . .
O1 O 0.76616(19) 0.63066(11) 0.42677(10) 0.0150(3) Uani 1 1 d . . . . .
H1C H 0.864222 0.628139 0.452893 0.023 Uiso 1 1 d R U . . .
O2 O 0.44262(19) 0.52183(10) 0.59587(10) 0.0117(3) Uani 1 1 d . . . . .
O3 O 0.77762(19) 0.47336(11) 0.55697(10) 0.0130(3) Uani 1 1 d . . . . .
O4 O 0.58790(19) 0.35216(10) 0.54996(10) 0.0134(3) Uani 1 1 d . . . . .
O5 O 0.8474(2) 0.33346(11) 0.60791(11) 0.0173(3) Uani 1 1 d . . . . .
O6 O 0.0152(3) 0.43241(14) 0.75111(16) 0.0322(5) Uani 1 1 d D . . . .
O7 O 0.1679(2) 0.59761(14) 0.68393(13) 0.0237(4) Uani 1 1 d D . . . .
O8 O 0.0229(2) 0.72977(14) 0.56573(13) 0.0266(4) Uani 1 1 d . . . . .
H8C H 0.044757 0.787187 0.574484 0.032 Uiso 1 1 d R U . . .
H8A H 0.052337 0.713067 0.501384 0.032 Uiso 1 1 d R U . . .
O9 O 0.0538(4) 0.92105(19) 0.56548(19) 0.0605(7) Uani 1 1 d . . . . .
H9C H 0.157732 0.936139 0.558120 0.073 Uiso 1 1 d R U . . .
H9B H 0.018402 0.942799 0.616870 0.091 Uiso 1 1 d R U . . .
O10 O 0.6676(2) 0.17698(13) 0.66356(13) 0.0230(4) Uani 1 1 d D . . . .
H1 H -0.037(5) 0.407(3) 0.707(2) 0.053(12) Uiso 1 1 d D . . . .
H2 H 0.057(5) 0.483(2) 0.730(3) 0.067(14) Uiso 1 1 d D . . . .
H3 H 0.243(3) 0.572(2) 0.653(2) 0.030(9) Uiso 1 1 d D . . . .
H4 H 0.129(5) 0.641(2) 0.650(3) 0.062(13) Uiso 1 1 d D . . . .
H9 H 0.723(4) 0.220(2) 0.641(3) 0.051(11) Uiso 1 1 d D . . . .
H10 H 0.721(5) 0.156(3) 0.708(2) 0.058(12) Uiso 1 1 d D . . . .
O11 O 0.385(4) 0.9506(14) 0.4745(6) 0.064(4) Uani 0.61(6) 1 d . . . . .
O11' O 0.303(4) 0.9745(11) 0.4672(7) 0.056(5) Uani 0.53(6) 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
Ru1 O2 1.8878(15) . ?
Ru1 O2 1.9243(15) 3_666 ?
Ru1 O1 1.9925(15) . ?
Ru1 O4 2.0414(15) 3_666 ?
Ru1 O3 2.0441(15) . ?
Ru1 N1 2.1611(18) . ?
Ru1 Ru1 2.3897(3) 3_666 ?
N1 C3 1.484(3) . ?
N1 C2 1.486(3) . ?
N1 H1B 0.9000 . ?
N2 C5 1.494(3) . ?
N2 C4 1.501(3) . ?
N2 H2D 0.8999 . ?
N2 H2C 0.9000 . ?
C1 O5 1.261(3) . ?
C1 O3 1.298(3) . ?
C1 O4 1.304(3) . ?
C2 C4 1.526(3) . ?
C2 H2A 0.9601 . ?
C2 H2B 0.9599 . ?
C3 C5 1.517(3) . ?
C3 H3A 0.9602 . ?
C3 H3B 0.9600 . ?
C4 C6 1.516(3) . ?
C4 H4A 0.9599 . ?
C5 C7 1.517(3) . ?
C5 H5A 0.9600 . ?
C6 H6A 0.9599 . ?
C6 H6B 0.9599 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9599 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9601 . ?
O1 H1C 0.8501 . ?
O6 H1 0.835(19) . ?
O6 H2 0.852(19) . ?
O7 H3 0.827(18) . ?
O7 H4 0.841(19) . ?
O8 H8C 0.8502 . ?
O8 H8A 0.9835 . ?
O9 H9C 0.8501 . ?
O9 H9B 0.8500 . ?
O10 H9 0.826(19) . ?
O10 H10 0.818(19) . ?

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
O2 Ru1 O2 102.37(5) . 3_666 ?
O2 Ru1 O1 168.32(6) . . ?
O2 Ru1 O1 89.05(6) 3_666 . ?
O2 Ru1 O4 89.62(6) . 3_666 ?
O2 Ru1 O4 88.55(6) 3_666 3_666 ?
O1 Ru1 O4 88.19(6) . 3_666 ?
O2 Ru1 O3 89.79(6) . . ?
O2 Ru1 O3 88.46(6) 3_666 . ?
O1 Ru1 O3 93.02(6) . . ?
O4 Ru1 O3 176.76(6) 3_666 . ?
O2 Ru1 N1 85.22(7) . . ?
O2 Ru1 N1 172.31(7) 3_666 . ?
O1 Ru1 N1 83.43(7) . . ?
O4 Ru1 N1 92.79(6) 3_666 . ?
O3 Ru1 N1 90.34(7) . . ?
O2 Ru1 Ru1 51.87(4) . 3_666 ?
O2 Ru1 Ru1 50.50(4) 3_666 3_666 ?
O1 Ru1 Ru1 139.48(5) . 3_666 ?
O4 Ru1 Ru1 88.53(4) 3_666 3_666 ?
O3 Ru1 Ru1 88.59(4) . 3_666 ?
N1 Ru1 Ru1 137.07(5) . 3_666 ?
C3 N1 C2 110.39(17) . . ?
C3 N1 Ru1 112.36(13) . . ?
C2 N1 Ru1 115.01(13) . . ?
C3 N1 H1B 106.1 . . ?
C2 N1 H1B 106.1 . . ?
Ru1 N1 H1B 106.2 . . ?
C5 N2 C4 111.89(17) . . ?
C5 N2 H2D 108.7 . . ?
C4 N2 H2D 108.7 . . ?
C5 N2 H2C 109.3 . . ?
C4 N2 H2C 109.3 . . ?
H2D N2 H2C 108.9 . . ?
O5 C1 O3 118.75(19) . . ?
O5 C1 O4 118.1(2) . . ?
O3 C1 O4 123.11(19) . . ?
N1 C2 C4 113.37(18) . . ?
N1 C2 H2A 108.6 . . ?
C4 C2 H2A 108.7 . . ?
N1 C2 H2B 109.1 . . ?
C4 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 C5 113.34(18) . . ?
N1 C3 H3A 109.1 . . ?
C5 C3 H3A 109.2 . . ?
N1 C3 H3B 108.6 . . ?
C5 C3 H3B 108.6 . . ?
H3A C3 H3B 107.8 . . ?
N2 C4 C6 109.04(18) . . ?
N2 C4 C2 109.40(17) . . ?
C6 C4 C2 111.50(19) . . ?
N2 C4 H4A 108.9 . . ?
C6 C4 H4A 109.0 . . ?
C2 C4 H4A 108.9 . . ?
N2 C5 C7 109.81(19) . . ?
N2 C5 C3 108.78(18) . . ?
C7 C5 C3 111.13(19) . . ?
N2 C5 H5A 109.0 . . ?
C7 C5 H5A 109.3 . . ?
C3 C5 H5A 108.8 . . ?
C4 C6 H6A 109.6 . . ?
C4 C6 H6B 109.6 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.2 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.6 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.4 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Ru1 O1 H1C 109.3 . . ?
Ru1 O2 Ru1 77.63(5) . 3_666 ?
C1 O3 Ru1 119.78(13) . . ?
C1 O4 Ru1 119.87(13) . 3_666 ?
H1 O6 H2 107(4) . . ?
H3 O7 H4 106(4) . . ?
H8C O8 H8A 109.0 . . ?
H9C O9 H9B 109.8 . . ?
H9 O10 H10 108(4) . . ?

_refine_diff_density_max         0.546
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.094

####################################################################### 
# 
# 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_I4m
_database_code_depnum_ccdc_archive 'CCDC 2308509'
loop_
_audit_author_name
_audit_author_address
'Bin Liu'
;Northwest University
China
;
_audit_update_record             
;
2023-12-21 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_I4m                 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.913 Why? 
RESPONSE: low crystal quality leading to poor diffraction data
;
_vrf_PLAT911_I4m                 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.596 21 Report
RESPONSE: low crystal quality leading to poor diffraction data
;
_vrf_PLAT971_I4m                 
;
PROBLEM: Check Calcd Resid. Dens. 0.86Ang From Ru1 3.32 eA-3 
RESPONSE: low crystal quality leading to poor diffraction data
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl10 O Ru2, 4 K'
_chemical_formula_sum            'Cl10 K4 O Ru2'
_chemical_formula_weight         729.04

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'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'

_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, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z'
'y, x, -z'
'-x, y, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z'
'-y, -x, z'
'x, -y, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   7.1221(11)
_cell_length_b                   7.1221(11)
_cell_length_c                   17.185(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     871.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1386
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      28.86

_exptl_crystal_description       block
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.778
_exptl_crystal_F_000             684
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    4.197
_shelx_estimated_absorpt_T_min   0.313
_shelx_estimated_absorpt_T_max   0.487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_T_max  0.480
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2008
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.370
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_full        25.048
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measured_fraction_theta_full 0.913
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_Laue_measured_fraction_full 0.913
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_point_group_measured_fraction_full 0.913
_reflns_number_total             240
_reflns_number_gt                218
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0391P)²+22.5548P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         240
_refine_ls_number_parameters     20
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0912
_refine_ls_wR_factor_gt          0.0876
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 1.000000 0.000000 0.39404(8) 0.0242(4) Uani 1 8 d S T P . .
Cl1 Cl 0.7655(2) 0.2345(2) 0.38669(14) 0.0330(6) Uani 1 2 d S T P . .
Cl2 Cl 1.000000 0.000000 0.2600(3) 0.0421(12) Uani 1 8 d S T P . .
O1 O 1.000000 0.000000 0.500000 0.023(3) Uani 1 16 d S T P . .
K1 K 1.000000 0.500000 0.250000 0.0509(12) Uani 1 8 d S T P . .
K2 K 1.000000 0.500000 0.500000 0.0403(10) Uani 1 8 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
Ru1 O1 1.8209(15) . ?
Ru1 Cl2 2.304(5) . ?
Ru1 Cl1 2.365(2) . ?
Ru1 Cl1 2.365(2) 2_645 ?
Ru1 Cl1 2.365(2) 4_665 ?
Ru1 Cl1 2.365(2) 3_755 ?
Ru1 K2 3.9996(8) 2_745 ?
Ru1 K2 3.9996(8) . ?
Ru1 K2 3.9996(8) 1_545 ?
Ru1 K2 3.9996(8) 2_645 ?
Cl1 K2 3.1870(15) . ?
Cl1 K2 3.1870(15) 2_645 ?
Cl1 K1 3.4471(17) 25_655 ?
Cl1 K1 3.4471(17) . ?
Cl2 K1 3.5652(6) 25_655 ?
Cl2 K1 3.5652(6) 1_545 ?
Cl2 K1 3.5652(6) 25_755 ?
Cl2 K1 3.5652(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ru1 Cl2 180.0 . . ?
O1 Ru1 Cl1 93.06(6) . . ?
Cl2 Ru1 Cl1 86.94(6) . . ?
O1 Ru1 Cl1 93.06(6) . 2_645 ?
Cl2 Ru1 Cl1 86.94(6) . 2_645 ?
Cl1 Ru1 Cl1 89.836(7) . 2_645 ?
O1 Ru1 Cl1 93.06(6) . 4_665 ?
Cl2 Ru1 Cl1 86.94(6) . 4_665 ?
Cl1 Ru1 Cl1 89.836(7) . 4_665 ?
Cl1 Ru1 Cl1 173.87(13) 2_645 4_665 ?
O1 Ru1 Cl1 93.06(6) . 3_755 ?
Cl2 Ru1 Cl1 86.94(6) . 3_755 ?
Cl1 Ru1 Cl1 173.87(13) . 3_755 ?
Cl1 Ru1 Cl1 89.836(7) 2_645 3_755 ?
Cl1 Ru1 Cl1 89.836(7) 4_665 3_755 ?
O1 Ru1 K2 62.92(2) . 2_745 ?
Cl2 Ru1 K2 117.08(2) . 2_745 ?
Cl1 Ru1 K2 130.77(4) . 2_745 ?
Cl1 Ru1 K2 130.77(4) 2_645 2_745 ?
Cl1 Ru1 K2 52.82(4) 4_665 2_745 ?
Cl1 Ru1 K2 52.82(4) 3_755 2_745 ?
O1 Ru1 K2 62.92(2) . . ?
Cl2 Ru1 K2 117.08(2) . . ?
Cl1 Ru1 K2 52.82(4) . . ?
Cl1 Ru1 K2 130.77(4) 2_645 . ?
Cl1 Ru1 K2 52.82(4) 4_665 . ?
Cl1 Ru1 K2 130.77(4) 3_755 . ?
K2 Ru1 K2 78.038(16) 2_745 . ?
O1 Ru1 K2 62.918(19) . 1_545 ?
Cl2 Ru1 K2 117.082(19) . 1_545 ?
Cl1 Ru1 K2 130.77(4) . 1_545 ?
Cl1 Ru1 K2 52.82(4) 2_645 1_545 ?
Cl1 Ru1 K2 130.77(4) 4_665 1_545 ?
Cl1 Ru1 K2 52.82(4) 3_755 1_545 ?
K2 Ru1 K2 78.038(16) 2_745 1_545 ?
K2 Ru1 K2 125.84(4) . 1_545 ?
O1 Ru1 K2 62.918(19) . 2_645 ?
Cl2 Ru1 K2 117.082(19) . 2_645 ?
Cl1 Ru1 K2 52.82(4) . 2_645 ?
Cl1 Ru1 K2 52.82(4) 2_645 2_645 ?
Cl1 Ru1 K2 130.77(4) 4_665 2_645 ?
Cl1 Ru1 K2 130.77(4) 3_755 2_645 ?
K2 Ru1 K2 125.84(4) 2_745 2_645 ?
K2 Ru1 K2 78.038(16) . 2_645 ?
K2 Ru1 K2 78.038(16) 1_545 2_645 ?
Ru1 Cl1 K2 90.93(5) . . ?
Ru1 Cl1 K2 90.93(5) . 2_645 ?
K2 Cl1 K2 104.39(7) . 2_645 ?
Ru1 Cl1 K1 94.68(6) . 25_655 ?
K2 Cl1 K1 172.43(7) . 25_655 ?
K2 Cl1 K1 80.618(16) 2_645 25_655 ?
Ru1 Cl1 K1 94.68(6) . . ?
K2 Cl1 K1 80.618(16) . . ?
K2 Cl1 K1 172.43(7) 2_645 . ?
K1 Cl1 K1 93.85(6) 25_655 . ?
Ru1 Cl2 K1 92.76(8) . 25_655 ?
Ru1 Cl2 K1 92.76(8) . 1_545 ?
K1 Cl2 K1 89.867(7) 25_655 1_545 ?
Ru1 Cl2 K1 92.76(8) . 25_755 ?
K1 Cl2 K1 174.48(15) 25_655 25_755 ?
K1 Cl2 K1 89.867(7) 1_545 25_755 ?
Ru1 Cl2 K1 92.76(8) . . ?
K1 Cl2 K1 89.867(7) 25_655 . ?
K1 Cl2 K1 174.48(15) 1_545 . ?
K1 Cl2 K1 89.867(7) 25_755 . ?
Ru1 O1 Ru1 180.0 17_756 . ?
Cl1 K1 Cl1 174.81(7) 3_765 25_655 ?
Cl1 K1 Cl1 117.67(3) 3_765 28_645 ?
Cl1 K1 Cl1 66.54(7) 25_655 28_645 ?
Cl1 K1 Cl1 66.54(7) 3_765 4_665 ?
Cl1 K1 Cl1 117.67(3) 25_655 4_665 ?
Cl1 K1 Cl1 86.15(6) 28_645 4_665 ?
Cl1 K1 Cl1 117.67(3) 3_765 26_565 ?
Cl1 K1 Cl1 57.96(6) 25_655 26_565 ?
Cl1 K1 Cl1 94.09(6) 28_645 26_565 ?
Cl1 K1 Cl1 174.81(7) 4_665 26_565 ?
Cl1 K1 Cl1 57.96(6) 3_765 2_655 ?
Cl1 K1 Cl1 117.67(3) 25_655 2_655 ?
Cl1 K1 Cl1 174.81(7) 28_645 2_655 ?
Cl1 K1 Cl1 94.09(6) 4_665 2_655 ?
Cl1 K1 Cl1 86.15(6) 26_565 2_655 ?
Cl1 K1 Cl1 86.15(6) 3_765 27 ?
Cl1 K1 Cl1 94.09(6) 25_655 27 ?
Cl1 K1 Cl1 57.96(6) 28_645 27 ?
Cl1 K1 Cl1 117.67(3) 4_665 27 ?
Cl1 K1 Cl1 66.54(7) 26_565 27 ?
Cl1 K1 Cl1 117.67(3) 2_655 27 ?
Cl1 K1 Cl1 94.09(6) 3_765 . ?
Cl1 K1 Cl1 86.15(6) 25_655 . ?
Cl1 K1 Cl1 117.67(3) 28_645 . ?
Cl1 K1 Cl1 57.96(6) 4_665 . ?
Cl1 K1 Cl1 117.67(3) 26_565 . ?
Cl1 K1 Cl1 66.54(7) 2_655 . ?
Cl1 K1 Cl1 174.81(7) 27 . ?
Cl1 K1 Cl2 121.11(6) 3_765 25_655 ?
Cl1 K1 Cl2 54.50(7) 25_655 25_655 ?
Cl1 K1 Cl2 121.01(7) 28_645 25_655 ?
Cl1 K1 Cl2 121.11(6) 4_665 25_655 ?
Cl1 K1 Cl2 54.50(7) 26_565 25_655 ?
Cl1 K1 Cl2 63.18(7) 2_655 25_655 ?
Cl1 K1 Cl2 121.01(7) 27 25_655 ?
Cl1 K1 Cl2 63.18(7) . 25_655 ?
Cl1 K1 Cl2 54.50(7) 3_765 1_565 ?
Cl1 K1 Cl2 121.11(6) 25_655 1_565 ?
Cl1 K1 Cl2 121.11(6) 28_645 1_565 ?
Cl1 K1 Cl2 121.01(7) 4_665 1_565 ?
Cl1 K1 Cl2 63.18(7) 26_565 1_565 ?
Cl1 K1 Cl2 54.50(7) 2_655 1_565 ?
Cl1 K1 Cl2 63.18(7) 27 1_565 ?
Cl1 K1 Cl2 121.01(7) . 1_565 ?
Cl2 K1 Cl2 90.133(7) 25_655 1_565 ?
Cl1 K1 Cl2 63.18(7) 3_765 25_755 ?
Cl1 K1 Cl2 121.01(7) 25_655 25_755 ?
Cl1 K1 Cl2 54.50(7) 28_645 25_755 ?
Cl1 K1 Cl2 63.18(7) 4_665 25_755 ?
Cl1 K1 Cl2 121.01(7) 26_565 25_755 ?
Cl1 K1 Cl2 121.11(6) 2_655 25_755 ?
Cl1 K1 Cl2 54.50(7) 27 25_755 ?
Cl1 K1 Cl2 121.11(6) . 25_755 ?
Cl2 K1 Cl2 174.48(15) 25_655 25_755 ?
Cl2 K1 Cl2 90.133(8) 1_565 25_755 ?
Cl1 K1 Cl2 121.00(7) 3_765 . ?
Cl1 K1 Cl2 63.18(7) 25_655 . ?
Cl1 K1 Cl2 63.18(7) 28_645 . ?
Cl1 K1 Cl2 54.50(7) 4_665 . ?
Cl1 K1 Cl2 121.11(6) 26_565 . ?
Cl1 K1 Cl2 121.00(7) 2_655 . ?
Cl1 K1 Cl2 121.11(6) 27 . ?
Cl1 K1 Cl2 54.50(7) . . ?
Cl2 K1 Cl2 90.133(7) 25_655 . ?
Cl2 K1 Cl2 174.48(15) 1_565 . ?
Cl2 K1 Cl2 90.133(7) 25_755 . ?
Cl1 K2 Cl1 180.0 . 17_766 ?
Cl1 K2 Cl1 116.79(7) . 20_656 ?
Cl1 K2 Cl1 63.21(7) 17_766 20_656 ?
Cl1 K2 Cl1 63.21(7) . 4_665 ?
Cl1 K2 Cl1 116.79(7) 17_766 4_665 ?
Cl1 K2 Cl1 180.00(7) 20_656 4_665 ?
Cl1 K2 Cl1 107.21(7) . 18_666 ?
Cl1 K2 Cl1 72.79(7) 17_766 18_666 ?
Cl1 K2 Cl1 104.67(7) 20_656 18_666 ?
Cl1 K2 Cl1 75.33(7) 4_665 18_666 ?
Cl1 K2 Cl1 72.79(7) . 2_655 ?
Cl1 K2 Cl1 107.21(7) 17_766 2_655 ?
Cl1 K2 Cl1 75.33(7) 20_656 2_655 ?
Cl1 K2 Cl1 104.67(7) 4_665 2_655 ?
Cl1 K2 Cl1 180.00(7) 18_666 2_655 ?
Cl1 K2 Cl1 75.32(7) . 19_556 ?
Cl1 K2 Cl1 104.67(7) 17_766 19_556 ?
Cl1 K2 Cl1 72.79(7) 20_656 19_556 ?
Cl1 K2 Cl1 107.21(7) 4_665 19_556 ?
Cl1 K2 Cl1 63.21(7) 18_666 19_556 ?
Cl1 K2 Cl1 116.79(7) 2_655 19_556 ?
Cl1 K2 Cl1 104.68(7) . 3_765 ?
Cl1 K2 Cl1 75.33(7) 17_766 3_765 ?
Cl1 K2 Cl1 107.21(7) 20_656 3_765 ?
Cl1 K2 Cl1 72.79(7) 4_665 3_765 ?
Cl1 K2 Cl1 116.79(7) 18_666 3_765 ?
Cl1 K2 Cl1 63.21(7) 2_655 3_765 ?
Cl1 K2 Cl1 180.0 19_556 3_765 ?
Cl1 K2 Ru1 36.25(4) . . ?
Cl1 K2 Ru1 143.75(4) 17_766 . ?
Cl1 K2 Ru1 143.75(4) 20_656 . ?
Cl1 K2 Ru1 36.25(4) 4_665 . ?
Cl1 K2 Ru1 75.52(4) 18_666 . ?
Cl1 K2 Ru1 104.48(4) 2_655 . ?
Cl1 K2 Ru1 75.52(4) 19_556 . ?
Cl1 K2 Ru1 104.48(4) 3_765 . ?
Cl1 K2 Ru1 143.75(4) . 17_766 ?
Cl1 K2 Ru1 36.25(4) 17_766 17_766 ?
Cl1 K2 Ru1 36.25(4) 20_656 17_766 ?
Cl1 K2 Ru1 143.75(4) 4_665 17_766 ?
Cl1 K2 Ru1 104.48(4) 18_666 17_766 ?
Cl1 K2 Ru1 75.52(4) 2_655 17_766 ?
Cl1 K2 Ru1 104.48(4) 19_556 17_766 ?
Cl1 K2 Ru1 75.52(4) 3_765 17_766 ?
Ru1 K2 Ru1 180.0 . 17_766 ?
Cl1 K2 Ru1 104.48(4) . 1_565 ?
Cl1 K2 Ru1 75.52(4) 17_766 1_565 ?
Cl1 K2 Ru1 75.52(4) 20_656 1_565 ?
Cl1 K2 Ru1 104.48(4) 4_665 1_565 ?
Cl1 K2 Ru1 143.75(4) 18_666 1_565 ?
Cl1 K2 Ru1 36.25(4) 2_655 1_565 ?
Cl1 K2 Ru1 143.75(4) 19_556 1_565 ?
Cl1 K2 Ru1 36.25(4) 3_765 1_565 ?
Ru1 K2 Ru1 125.84(4) . 1_565 ?
Ru1 K2 Ru1 54.16(4) 17_766 1_565 ?
Cl1 K2 Ru1 75.52(4) . 17_756 ?
Cl1 K2 Ru1 104.48(4) 17_766 17_756 ?
Cl1 K2 Ru1 104.48(4) 20_656 17_756 ?
Cl1 K2 Ru1 75.52(4) 4_665 17_756 ?
Cl1 K2 Ru1 36.25(4) 18_666 17_756 ?
Cl1 K2 Ru1 143.75(4) 2_655 17_756 ?
Cl1 K2 Ru1 36.25(4) 19_556 17_756 ?
Cl1 K2 Ru1 143.75(4) 3_765 17_756 ?
Ru1 K2 Ru1 54.16(4) . 17_756 ?
Ru1 K2 Ru1 125.84(4) 17_766 17_756 ?
Ru1 K2 Ru1 180.0 1_565 17_756 ?

_refine_diff_density_max         3.193
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.181

####################################################################### 
# 
# 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_xb0614_0m
_database_code_depnum_ccdc_archive 'CCDC 2003395'
loop_
_audit_author_name
_audit_author_address
'Bin Liu'
;Northwest University
China
;
_audit_update_record             
;
2023-12-21 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_xb0614_0m           
;
PROBLEM: D-H Bond Without Acceptor O5 --H1 . Please Check 
RESPONSE: constraint hydrogen treatment resulted in the Alert level B problem
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H2O Ni2 O20 Ru2, 2(H2 O)'
_chemical_formula_sum            'C2 H24 Ni2 O22 Ru2'
_chemical_formula_weight         719.77

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'
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'
Ni Ni 0.3393 1.1124 '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'

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

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

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

_cell_length_a                   9.2137(9)
_cell_length_b                   5.9918(6)
_cell_length_c                   16.2072(15)
_cell_angle_alpha                90
_cell_angle_beta                 96.8500(10)
_cell_angle_gamma                90
_cell_volume                     888.36(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2720
_cell_measurement_theta_min      3.16
_cell_measurement_theta_max      26.89

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.691
_exptl_crystal_F_000             712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    3.866
_shelx_estimated_absorpt_T_min   0.433
_shelx_estimated_absorpt_T_max   0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.415
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4778
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.226
_diffrn_reflns_theta_max         26.893
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1878
_reflns_number_gt                1737
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0235P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1878
_refine_ls_number_parameters     172
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0176
_refine_ls_wR_factor_ref         0.0436
_refine_ls_wR_factor_gt          0.0428
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.080
_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
Ru1 Ru 0.58185(2) 0.06340(3) 0.45331(2) 0.01541(7) Uani 1 1 d . . . . .
Ni1 Ni 0.75689(3) 0.28121(5) 0.31775(2) 0.01641(9) Uani 1 1 d . . . . .
C1 C 0.2886(3) 0.2575(4) 0.42396(15) 0.0201(5) Uani 1 1 d . . . . .
O1 O 0.26263(17) 0.1440(3) 0.48866(10) 0.0232(4) Uani 1 1 d . . . . .
O2 O 0.41781(17) 0.2624(3) 0.39879(10) 0.0228(4) Uani 1 1 d . . . . .
O3 O 0.45058(17) -0.1796(3) 0.44147(10) 0.0199(4) Uani 1 1 d . . . . .
O4 O 0.18690(18) 0.3659(3) 0.38513(12) 0.0292(4) Uani 1 1 d . . . . .
O5 O 0.73852(17) 0.3047(3) 0.44353(10) 0.0192(4) Uani 1 1 d . . . . .
O6 O 0.63593(18) 0.0008(3) 0.33682(10) 0.0188(4) Uani 1 1 d D . . . .
O7 O 0.8781(2) 0.5672(3) 0.31002(13) 0.0269(4) Uani 1 1 d D . . . .
O8 O 0.7613(2) 0.2423(3) 0.19336(11) 0.0245(4) Uani 1 1 d D . . . .
O9 O 0.57451(19) 0.4860(3) 0.29602(12) 0.0247(4) Uani 1 1 d D . . . .
O10 O 0.95574(19) 0.1111(3) 0.33493(12) 0.0240(4) Uani 1 1 d D . . . .
O11 O -0.0004(2) 0.7668(3) 0.44868(12) 0.0273(4) Uani 1 1 d D . . . .
H1 H 0.705921 0.434886 0.461737 0.047(10) Uiso 1 1 d R . . . .
H2 H 0.677(3) -0.116(3) 0.3331(16) 0.020(7) Uiso 1 1 d D . . . .
H3 H 0.920(4) 0.613(6) 0.3528(15) 0.056(12) Uiso 1 1 d D . . . .
H4 H 0.917(3) 0.597(5) 0.2681(14) 0.041(10) Uiso 1 1 d D . . . .
H5 H 0.693(3) 0.287(5) 0.1592(18) 0.050(10) Uiso 1 1 d D . . . .
H6 H 0.781(4) 0.119(4) 0.176(2) 0.046(10) Uiso 1 1 d D . . . .
H7 H 0.514(3) 0.442(5) 0.3260(16) 0.035(9) Uiso 1 1 d D . . . .
H8 H 0.524(3) 0.509(5) 0.2516(14) 0.040(10) Uiso 1 1 d D . . . .
H9 H 0.963(3) 0.003(4) 0.3664(15) 0.027(8) Uiso 1 1 d D . . . .
H10 H 1.021(3) 0.208(5) 0.347(2) 0.053(11) Uiso 1 1 d D . . . .
H11 H -0.065(2) 0.776(5) 0.4757(16) 0.028(8) Uiso 1 1 d D . . . .
H12 H 0.077(2) 0.745(5) 0.4778(17) 0.038(9) Uiso 1 1 d 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
Ru1 O3 1.8880(16) . ?
Ru1 O3 1.8983(16) 3_656 ?
Ru1 O1 2.0396(17) 3_656 ?
Ru1 O2 2.0416(16) . ?
Ru1 O6 2.0439(16) . ?
Ru1 O5 2.0624(16) . ?
Ru1 Ru1 2.3848(4) 3_656 ?
Ni1 O8 2.0347(18) . ?
Ni1 O7 2.0575(19) . ?
Ni1 O6 2.0597(17) . ?
Ni1 O5 2.0704(16) . ?
Ni1 O9 2.0767(18) . ?
Ni1 O10 2.0860(18) . ?
C1 O4 1.247(3) . ?
C1 O1 1.296(3) . ?
C1 O2 1.304(3) . ?
O5 H1 0.8984 . ?
O6 H2 0.802(17) . ?
O7 H3 0.803(18) . ?
O7 H4 0.823(18) . ?
O8 H5 0.832(18) . ?
O8 H6 0.815(18) . ?
O9 H7 0.826(17) . ?
O9 H8 0.821(18) . ?
O10 H9 0.823(17) . ?
O10 H10 0.840(18) . ?
O11 H11 0.784(17) . ?
O11 H12 0.820(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ru1 O3 101.92(6) . 3_656 ?
O3 Ru1 O1 89.05(7) . 3_656 ?
O3 Ru1 O1 89.22(7) 3_656 3_656 ?
O3 Ru1 O2 88.52(7) . . ?
O3 Ru1 O2 89.25(7) 3_656 . ?
O1 Ru1 O2 176.80(6) 3_656 . ?
O3 Ru1 O6 89.34(7) . . ?
O3 Ru1 O6 168.21(7) 3_656 . ?
O1 Ru1 O6 94.53(7) 3_656 . ?
O2 Ru1 O6 87.53(7) . . ?
O3 Ru1 O5 168.12(6) . . ?
O3 Ru1 O5 89.92(7) 3_656 . ?
O1 Ru1 O5 90.16(7) 3_656 . ?
O2 Ru1 O5 92.65(7) . . ?
O6 Ru1 O5 78.91(7) . . ?
O3 Ru1 Ru1 51.15(5) . 3_656 ?
O3 Ru1 Ru1 50.77(5) 3_656 3_656 ?
O1 Ru1 Ru1 88.62(5) 3_656 3_656 ?
O2 Ru1 Ru1 88.23(5) . 3_656 ?
O6 Ru1 Ru1 140.36(5) . 3_656 ?
O5 Ru1 Ru1 140.67(5) . 3_656 ?
O8 Ni1 O7 87.72(8) . . ?
O8 Ni1 O6 97.48(7) . . ?
O7 Ni1 O6 174.80(7) . . ?
O8 Ni1 O5 175.57(7) . . ?
O7 Ni1 O5 96.43(7) . . ?
O6 Ni1 O5 78.37(6) . . ?
O8 Ni1 O9 90.64(8) . . ?
O7 Ni1 O9 86.07(8) . . ?
O6 Ni1 O9 93.79(7) . . ?
O5 Ni1 O9 88.12(7) . . ?
O8 Ni1 O10 87.44(8) . . ?
O7 Ni1 O10 86.60(8) . . ?
O6 Ni1 O10 93.66(7) . . ?
O5 Ni1 O10 94.32(7) . . ?
O9 Ni1 O10 172.49(8) . . ?
O4 C1 O1 118.8(2) . . ?
O4 C1 O2 119.3(2) . . ?
O1 C1 O2 121.9(2) . . ?
C1 O1 Ru1 120.36(15) . 3_656 ?
C1 O2 Ru1 120.52(15) . . ?
Ru1 O3 Ru1 78.08(6) . 3_656 ?
Ru1 O5 Ni1 99.68(7) . . ?
Ru1 O5 H1 108.6 . . ?
Ni1 O5 H1 116.9 . . ?
Ru1 O6 Ni1 100.65(7) . . ?
Ru1 O6 H2 113.5(19) . . ?
Ni1 O6 H2 115.8(19) . . ?
Ni1 O7 H3 116(3) . . ?
Ni1 O7 H4 122(2) . . ?
H3 O7 H4 115(3) . . ?
Ni1 O8 H5 121(2) . . ?
Ni1 O8 H6 118(2) . . ?
H5 O8 H6 104(3) . . ?
Ni1 O9 H7 108(2) . . ?
Ni1 O9 H8 127(2) . . ?
H7 O9 H8 103(3) . . ?
Ni1 O10 H9 118(2) . . ?
Ni1 O10 H10 107(2) . . ?
H9 O10 H10 113(3) . . ?
H11 O11 H12 111(3) . . ?

_refine_diff_density_max         0.387
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.079

####################################################################### 
# 
# 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_RuCl
_database_code_depnum_ccdc_archive 'CCDC 2308508'
loop_
_audit_author_name
_audit_author_address
'Bin Liu'
;Northwest University
China
;
_audit_update_record             
;
2023-12-21 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl5 H2 O Ru, 2 K'
_chemical_formula_sum            'Cl5 H2 K2 O Ru'
_chemical_formula_weight         374.54

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'
K K 0.2009 0.2494 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   13.5704(17)
_cell_length_b                   9.6330(12)
_cell_length_c                   7.0067(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     915.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1459
_cell_measurement_theta_min      3.272
_cell_measurement_theta_max      27.06

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.716
_exptl_crystal_F_000             708
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    4.002
_shelx_estimated_absorpt_T_min   0.380
_shelx_estimated_absorpt_T_max   0.533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_T_max  0.480
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5036
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.002
_diffrn_reflns_theta_max         27.342
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1092
_reflns_number_gt                899
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0397P)²+1.9654P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1092
_refine_ls_number_parameters     56
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0812
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

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 0.11011(3) 0.750000 0.19039(7) 0.02525(16) Uani 1 2 d S T P . .
Cl1 Cl 0.10768(9) 0.99560(11) 0.18894(18) 0.0416(3) Uani 1 1 d . . . . .
Cl2 Cl 0.00418(12) 0.750000 0.4580(3) 0.0435(4) Uani 1 2 d S T P . .
Cl4 Cl 0.21480(14) 0.750000 -0.0759(2) 0.0473(4) Uani 1 2 d S T P . .
Cl5 Cl 0.24622(11) 0.750000 0.3927(2) 0.0332(3) Uani 1 2 d S T P . .
O1 O -0.0134(4) 0.750000 0.0090(8) 0.0438(12) Uani 1 2 d DS T P . .
K1 K 0.14650(9) 1.00169(12) -0.35004(17) 0.0498(3) Uani 1 1 d . . . . .
H1 H 0.016(3) 0.750000 -0.095(5) 0.011(15) Uiso 1 2 d DS . P . .
H2 H -0.055(5) 0.683(7) 0.022(11) 0.05(3) Uiso 0.5 1 d D . 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
Ru1 O1 2.104(4) . ?
Ru1 Cl5 2.3284(14) . ?
Ru1 Cl4 2.3452(17) . ?
Ru1 Cl2 2.3628(17) . ?
Ru1 Cl1 2.3661(11) . ?
Ru1 Cl1 2.3661(11) 8_575 ?
Ru1 K1 4.0609(12) 1_556 ?
Ru1 K1 4.0609(12) 8_576 ?
Ru1 K1 4.0879(13) 2_575 ?
Ru1 K1 4.0879(13) 7_656 ?
Cl1 K1 3.2734(17) 1_556 ?
Cl1 K1 3.3472(18) 2_575 ?
Cl1 K1 3.6294(18) 5_575 ?
Cl2 K1 3.2365(16) 4_545 ?
Cl2 K1 3.2365(16) 5_575 ?
Cl2 K1 3.3789(17) 1_556 ?
Cl2 K1 3.3789(17) 8_576 ?
Cl4 K1 3.2291(16) . ?
Cl4 K1 3.2291(16) 8_575 ?
Cl4 K1 3.4305(18) 2_575 ?
Cl4 K1 3.4305(18) 7_656 ?
Cl5 K1 3.2763(15) 7_656 ?
Cl5 K1 3.2763(15) 2_575 ?
Cl5 K1 3.3103(16) 1_556 ?
Cl5 K1 3.3103(16) 8_576 ?
O1 H1 0.827(19) . ?
O1 H2 0.86(2) . ?
O1 H2 0.86(2) 8_575 ?
K1 K1 4.4906(16) 2_575 ?

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 Cl5 179.66(17) . . ?
O1 Ru1 Cl4 90.12(17) . . ?
Cl5 Ru1 Cl4 90.22(6) . . ?
O1 Ru1 Cl2 89.69(17) . . ?
Cl5 Ru1 Cl2 89.97(6) . . ?
Cl4 Ru1 Cl2 179.81(6) . . ?
O1 Ru1 Cl1 89.21(3) . . ?
Cl5 Ru1 Cl1 90.78(3) . . ?
Cl4 Ru1 Cl1 90.29(3) . . ?
Cl2 Ru1 Cl1 89.71(3) . . ?
O1 Ru1 Cl1 89.21(3) . 8_575 ?
Cl5 Ru1 Cl1 90.79(3) . 8_575 ?
Cl4 Ru1 Cl1 90.29(3) . 8_575 ?
Cl2 Ru1 Cl1 89.71(3) . 8_575 ?
Cl1 Ru1 Cl1 178.32(6) . 8_575 ?
O1 Ru1 K1 125.16(11) . 1_556 ?
Cl5 Ru1 K1 54.60(3) . 1_556 ?
Cl4 Ru1 K1 123.86(4) . 1_556 ?
Cl2 Ru1 K1 56.27(4) . 1_556 ?
Cl1 Ru1 K1 53.71(3) . 1_556 ?
Cl1 Ru1 K1 127.02(4) 8_575 1_556 ?
O1 Ru1 K1 125.16(11) . 8_576 ?
Cl5 Ru1 K1 54.60(3) . 8_576 ?
Cl4 Ru1 K1 123.86(4) . 8_576 ?
Cl2 Ru1 K1 56.27(4) . 8_576 ?
Cl1 Ru1 K1 127.02(4) . 8_576 ?
Cl1 Ru1 K1 53.71(3) 8_575 8_576 ?
K1 Ru1 K1 73.32(4) 1_556 8_576 ?
O1 Ru1 K1 127.01(11) . 2_575 ?
Cl5 Ru1 K1 53.22(3) . 2_575 ?
Cl4 Ru1 K1 57.00(4) . 2_575 ?
Cl2 Ru1 K1 123.13(4) . 2_575 ?
Cl1 Ru1 K1 54.96(4) . 2_575 ?
Cl1 Ru1 K1 126.59(4) 8_575 2_575 ?
K1 Ru1 K1 66.88(2) 1_556 2_575 ?
K1 Ru1 K1 107.82(2) 8_576 2_575 ?
O1 Ru1 K1 127.01(11) . 7_656 ?
Cl5 Ru1 K1 53.22(3) . 7_656 ?
Cl4 Ru1 K1 57.00(4) . 7_656 ?
Cl2 Ru1 K1 123.13(4) . 7_656 ?
Cl1 Ru1 K1 126.59(4) . 7_656 ?
Cl1 Ru1 K1 54.97(4) 8_575 7_656 ?
K1 Ru1 K1 107.82(2) 1_556 7_656 ?
K1 Ru1 K1 66.88(2) 8_576 7_656 ?
K1 Ru1 K1 71.63(3) 2_575 7_656 ?
Ru1 Cl1 K1 90.65(4) . 1_556 ?
Ru1 Cl1 K1 89.67(4) . 2_575 ?
K1 Cl1 K1 85.41(4) 1_556 2_575 ?
Ru1 Cl1 K1 91.10(4) . 5_575 ?
K1 Cl1 K1 81.14(4) 1_556 5_575 ?
K1 Cl1 K1 166.53(4) 2_575 5_575 ?
Ru1 Cl2 K1 101.47(5) . 4_545 ?
Ru1 Cl2 K1 101.47(5) . 5_575 ?
K1 Cl2 K1 95.30(6) 4_545 5_575 ?
Ru1 Cl2 K1 88.17(4) . 1_556 ?
K1 Cl2 K1 169.89(6) 4_545 1_556 ?
K1 Cl2 K1 85.63(3) 5_575 1_556 ?
Ru1 Cl2 K1 88.17(4) . 8_576 ?
K1 Cl2 K1 85.63(3) 4_545 8_576 ?
K1 Cl2 K1 169.89(6) 5_575 8_576 ?
K1 Cl2 K1 91.70(6) 1_556 8_576 ?
Ru1 Cl4 K1 107.42(5) . . ?
Ru1 Cl4 K1 107.42(5) . 8_575 ?
K1 Cl4 K1 97.32(6) . 8_575 ?
Ru1 Cl4 K1 88.02(4) . 2_575 ?
K1 Cl4 K1 84.74(2) . 2_575 ?
K1 Cl4 K1 162.83(6) 8_575 2_575 ?
Ru1 Cl4 K1 88.02(4) . 7_656 ?
K1 Cl4 K1 162.83(6) . 7_656 ?
K1 Cl4 K1 84.74(2) 8_575 7_656 ?
K1 Cl4 K1 88.42(6) 2_575 7_656 ?
Ru1 Cl5 K1 92.09(4) . 7_656 ?
Ru1 Cl5 K1 92.09(4) . 2_575 ?
K1 Cl5 K1 93.79(6) 7_656 2_575 ?
Ru1 Cl5 K1 90.41(4) . 1_556 ?
K1 Cl5 K1 177.50(5) 7_656 1_556 ?
K1 Cl5 K1 85.96(2) 2_575 1_556 ?
Ru1 Cl5 K1 90.41(4) . 8_576 ?
K1 Cl5 K1 85.96(2) 7_656 8_576 ?
K1 Cl5 K1 177.50(5) 2_575 8_576 ?
K1 Cl5 K1 94.18(6) 1_556 8_576 ?
Ru1 O1 H1 99(4) . . ?
Ru1 O1 H2 117(7) . . ?
H1 O1 H2 114(5) . . ?
Ru1 O1 H2 117(7) . 8_575 ?
H1 O1 H2 114(5) . 8_575 ?
H2 O1 H2 97(10) . 8_575 ?
Cl4 K1 Cl2 151.08(6) . 5_575 ?
Cl4 K1 Cl1 128.30(5) . 1_554 ?
Cl2 K1 Cl1 71.39(4) 5_575 1_554 ?
Cl4 K1 Cl5 96.42(4) . 2_574 ?
Cl2 K1 Cl5 82.10(4) 5_575 2_574 ?
Cl1 K1 Cl5 126.65(5) 1_554 2_574 ?
Cl4 K1 Cl5 69.92(4) . 1_554 ?
Cl2 K1 Cl5 132.24(5) 5_575 1_554 ?
Cl1 K1 Cl5 61.01(4) 1_554 1_554 ?
Cl5 K1 Cl5 129.47(4) 2_574 1_554 ?
Cl4 K1 Cl1 70.81(4) . 2_574 ?
Cl2 K1 Cl1 130.01(5) 5_575 2_574 ?
Cl1 K1 Cl1 103.95(5) 1_554 2_574 ?
Cl5 K1 Cl1 60.60(4) 2_574 2_574 ?
Cl5 K1 Cl1 69.07(4) 1_554 2_574 ?
Cl4 K1 Cl2 82.07(4) . 1_554 ?
Cl2 K1 Cl2 94.37(3) 5_575 1_554 ?
Cl1 K1 Cl2 60.16(4) 1_554 1_554 ?
Cl5 K1 Cl2 169.89(6) 2_574 1_554 ?
Cl5 K1 Cl2 59.43(4) 1_554 1_554 ?
Cl1 K1 Cl2 127.43(5) 2_574 1_554 ?
Cl4 K1 Cl4 129.82(4) . 2_574 ?
Cl2 K1 Cl4 73.95(4) 5_575 2_574 ?
Cl1 K1 Cl4 69.24(4) 1_554 2_574 ?
Cl5 K1 Cl4 59.11(4) 2_574 2_574 ?
Cl5 K1 Cl4 92.02(4) 1_554 2_574 ?
Cl1 K1 Cl4 59.03(4) 2_574 2_574 ?
Cl2 K1 Cl4 129.07(5) 1_554 2_574 ?
Cl4 K1 Cl1 95.35(5) . 5_575 ?
Cl2 K1 Cl1 57.79(4) 5_575 5_575 ?
Cl1 K1 Cl1 98.86(4) 1_554 5_575 ?
Cl5 K1 Cl1 104.81(4) 2_574 5_575 ?
Cl5 K1 Cl1 124.27(4) 1_554 5_575 ?
Cl1 K1 Cl1 157.18(4) 2_574 5_575 ?
Cl2 K1 Cl1 65.53(4) 1_554 5_575 ?
Cl4 K1 Cl1 131.29(5) 2_574 5_575 ?
Cl4 K1 Ru1 93.34(4) . 1_554 ?
Cl2 K1 Ru1 100.31(4) 5_575 1_554 ?
Cl1 K1 Ru1 35.64(2) 1_554 1_554 ?
Cl5 K1 Ru1 154.37(5) 2_574 1_554 ?
Cl5 K1 Ru1 34.99(3) 1_554 1_554 ?
Cl1 K1 Ru1 100.99(4) 2_574 1_554 ?
Cl2 K1 Ru1 35.56(3) 1_554 1_554 ?
Cl4 K1 Ru1 96.73(4) 2_574 1_554 ?
Cl1 K1 Ru1 97.78(3) 5_575 1_554 ?
Cl4 K1 Ru1 99.57(4) . 2_574 ?
Cl2 K1 Ru1 95.41(4) 5_575 2_574 ?
Cl1 K1 Ru1 102.06(4) 1_554 2_574 ?
Cl5 K1 Ru1 34.69(3) 2_574 2_574 ?
Cl5 K1 Ru1 97.82(4) 1_554 2_574 ?
Cl1 K1 Ru1 35.37(2) 2_574 2_574 ?
Cl2 K1 Ru1 155.40(5) 1_554 2_574 ?
Cl4 K1 Ru1 34.98(3) 2_574 2_574 ?
Cl1 K1 Ru1 137.91(4) 5_575 2_574 ?
Ru1 K1 Ru1 120.17(3) 1_554 2_574 ?
Cl4 K1 K1 49.53(3) . 2_575 ?
Cl2 K1 K1 125.66(5) 5_575 2_575 ?
Cl1 K1 K1 150.51(5) 1_554 2_575 ?
Cl5 K1 K1 47.34(3) 2_574 2_575 ?
Cl5 K1 K1 99.42(5) 1_554 2_575 ?
Cl1 K1 K1 46.60(4) 2_574 2_575 ?
Cl2 K1 K1 131.52(5) 1_554 2_575 ?
Cl4 K1 K1 91.24(5) 2_574 2_575 ?
Cl1 K1 K1 110.61(3) 5_575 2_575 ?
Ru1 K1 K1 133.66(4) 1_554 2_575 ?
Ru1 K1 K1 56.27(3) 2_574 2_575 ?

_refine_diff_density_max         1.457
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.126

####################################################################### 
# 
# 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_xb6856
_database_code_depnum_ccdc_archive 'CCDC 2003394'
loop_
_audit_author_name
_audit_author_address
'Bin Liu'
;Northwest University
China
;
_audit_update_record             
;
2023-12-21 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_xb6856              
;
PROBLEM: Short Inter D-H..H-D H7 ..H12 . 1.99 Ang. 
RESPONSE: constraint hydrogen_treatment resulted in the Alert level B problem
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H2O Mg2 O20 Ru2, 4(H2 O)'
_chemical_formula_sum            'C2 H28 Mg2 O24 Ru2'
_chemical_formula_weight         687.00

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'
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'
Mg Mg 0.0486 0.0363 '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'

_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                   7.7401(10)
_cell_length_b                   9.3154(12)
_cell_length_c                   14.1849(18)
_cell_angle_alpha                90
_cell_angle_beta                 98.067(2)
_cell_angle_gamma                90
_cell_volume                     1012.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3506
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      26.54

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_F_000             688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.665
_shelx_estimated_absorpt_T_min   0.635
_shelx_estimated_absorpt_T_max   0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5431
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.624
_diffrn_reflns_theta_max         26.567
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2091
_reflns_number_gt                1941
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0232P)²+0.6307P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2091
_refine_ls_number_parameters     192
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_ref         0.0511
_refine_ls_wR_factor_gt          0.0497
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.098
_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
Ru1 Ru 0.57863(2) 0.09569(2) 0.04349(2) 0.01806(7) Uani 1 1 d . . . . .
Mg1 Mg 0.80931(10) 0.33559(8) 0.16754(6) 0.02226(17) Uani 1 1 d . . . . .
C1 C 0.2143(3) 0.1632(2) -0.03618(17) 0.0232(5) Uani 1 1 d . . . . .
O1 O 0.2087(2) 0.03137(18) -0.06889(12) 0.0262(4) Uani 1 1 d . . . . .
O2 O 0.3545(2) 0.21712(17) 0.01339(12) 0.0257(4) Uani 1 1 d . . . . .
O3 O 0.5588(2) 0.05238(17) -0.08852(11) 0.0216(3) Uani 1 1 d . . . . .
O4 O 0.0811(2) 0.24026(18) -0.05520(13) 0.0298(4) Uani 1 1 d . . . . .
O5 O 0.6276(2) 0.17414(17) 0.18021(12) 0.0244(3) Uani 1 1 d D . . . .
O6 O 0.7382(2) 0.26567(17) 0.02613(11) 0.0231(3) Uani 1 1 d D . . . .
O7 O 0.8462(3) 0.3890(2) 0.31170(14) 0.0330(4) Uani 1 1 d D . . . .
O8 O 0.9807(3) 0.4902(2) 0.13542(15) 0.0370(4) Uani 1 1 d D . . . .
O9 O 0.6273(3) 0.4930(2) 0.15471(16) 0.0424(5) Uani 1 1 d D . . . .
O10 O 1.0199(3) 0.1996(2) 0.18602(16) 0.0374(4) Uani 1 1 d D . . . .
O11 O 0.2987(3) 0.0107(2) 0.57714(14) 0.0348(4) Uani 1 1 d D . . . .
O12 O 0.6445(3) 0.7656(2) 0.23331(15) 0.0392(5) Uani 1 1 d D . . . .
H1 H 0.665(4) 0.109(2) 0.2194(18) 0.043(9) Uiso 1 1 d D . . . .
H2 H 0.835(2) 0.240(3) 0.011(2) 0.040(9) Uiso 1 1 d D . . . .
H3 H 0.764(3) 0.404(3) 0.340(2) 0.051(11) Uiso 1 1 d D . . . .
H4 H 0.908(4) 0.340(3) 0.349(2) 0.050(10) Uiso 1 1 d D . . . .
H5 H 1.082(3) 0.477(4) 0.123(2) 0.048(10) Uiso 1 1 d D . . . .
H6 H 0.932(5) 0.558(3) 0.104(2) 0.066(12) Uiso 1 1 d D . . . .
H7 H 0.523(2) 0.488(3) 0.130(2) 0.038(8) Uiso 1 1 d D . . . .
H8 H 0.648(5) 0.574(3) 0.179(3) 0.071(13) Uiso 1 1 d D . . . .
H9 H 1.120(3) 0.226(4) 0.206(3) 0.069(12) Uiso 1 1 d D . . . .
H10 H 1.029(5) 0.114(2) 0.182(3) 0.068(13) Uiso 1 1 d D . . . .
H11 H 0.284(5) -0.053(3) 0.537(2) 0.067(12) Uiso 1 1 d D . . . .
H12 H 0.313(5) 0.084(3) 0.546(2) 0.059(12) Uiso 1 1 d D . . . .
H13 H 0.564(3) 0.748(4) 0.265(2) 0.056(11) Uiso 1 1 d D . . . .
H14 H 0.605(5) 0.829(3) 0.195(2) 0.076(13) Uiso 1 1 d 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
Ru1 O3 1.9006(16) . ?
Ru1 O3 1.9059(16) 3_655 ?
Ru1 O1 2.0186(16) 3_655 ?
Ru1 O6 2.0443(16) . ?
Ru1 O5 2.0572(16) . ?
Ru1 O2 2.0651(15) . ?
Ru1 Ru1 2.4002(4) 3_655 ?
Ru1 Mg1 3.2244(8) . ?
Mg1 O9 2.024(2) . ?
Mg1 O8 2.052(2) . ?
Mg1 O10 2.052(2) . ?
Mg1 O5 2.0841(18) . ?
Mg1 O7 2.085(2) . ?
Mg1 O6 2.1074(18) . ?
C1 O4 1.254(3) . ?
C1 O2 1.307(3) . ?
C1 O1 1.312(3) . ?
O5 H1 0.844(10) . ?
O6 H2 0.841(10) . ?
O7 H3 0.815(18) . ?
O7 H4 0.807(18) . ?
O8 H5 0.832(18) . ?
O8 H6 0.829(19) . ?
O9 H7 0.839(17) . ?
O9 H8 0.837(19) . ?
O10 H9 0.822(18) . ?
O10 H10 0.803(18) . ?
O11 H11 0.819(19) . ?
O11 H12 0.828(18) . ?
O12 H13 0.836(18) . ?
O12 H14 0.833(19) . ?

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
O3 Ru1 O3 101.82(6) . 3_655 ?
O3 Ru1 O1 90.14(7) . 3_655 ?
O3 Ru1 O1 89.74(7) 3_655 3_655 ?
O3 Ru1 O6 90.71(7) . . ?
O3 Ru1 O6 167.42(7) 3_655 . ?
O1 Ru1 O6 89.09(7) 3_655 . ?
O3 Ru1 O5 169.39(6) . . ?
O3 Ru1 O5 88.79(7) 3_655 . ?
O1 Ru1 O5 90.13(7) 3_655 . ?
O6 Ru1 O5 78.69(6) . . ?
O3 Ru1 O2 87.89(7) . . ?
O3 Ru1 O2 88.48(7) 3_655 . ?
O1 Ru1 O2 177.02(6) 3_655 . ?
O6 Ru1 O2 93.16(6) . . ?
O5 Ru1 O2 92.21(7) . . ?
O3 Ru1 Ru1 51.01(5) . 3_655 ?
O3 Ru1 Ru1 50.81(5) 3_655 3_655 ?
O1 Ru1 Ru1 89.91(5) 3_655 3_655 ?
O6 Ru1 Ru1 141.70(5) . 3_655 ?
O5 Ru1 Ru1 139.60(5) . 3_655 ?
O2 Ru1 Ru1 87.12(5) . 3_655 ?
O3 Ru1 Mg1 130.30(5) . . ?
O3 Ru1 Mg1 127.67(5) 3_655 . ?
O1 Ru1 Mg1 86.20(5) 3_655 . ?
O6 Ru1 Mg1 39.76(5) . . ?
O5 Ru1 Mg1 39.17(5) . . ?
O2 Ru1 Mg1 96.78(5) . . ?
Ru1 Ru1 Mg1 175.859(18) 3_655 . ?
O9 Mg1 O8 86.27(9) . . ?
O9 Mg1 O10 171.58(10) . . ?
O8 Mg1 O10 86.27(9) . . ?
O9 Mg1 O5 93.51(8) . . ?
O8 Mg1 O5 172.18(9) . . ?
O10 Mg1 O5 94.41(8) . . ?
O9 Mg1 O7 85.02(9) . . ?
O8 Mg1 O7 92.67(9) . . ?
O10 Mg1 O7 91.43(9) . . ?
O5 Mg1 O7 95.09(8) . . ?
O9 Mg1 O6 93.03(8) . . ?
O8 Mg1 O6 95.51(8) . . ?
O10 Mg1 O6 91.57(8) . . ?
O5 Mg1 O6 76.69(7) . . ?
O7 Mg1 O6 171.45(8) . . ?
O9 Mg1 Ru1 97.36(7) . . ?
O8 Mg1 Ru1 133.70(7) . . ?
O10 Mg1 Ru1 90.62(7) . . ?
O5 Mg1 Ru1 38.57(5) . . ?
O7 Mg1 Ru1 133.61(6) . . ?
O6 Mg1 Ru1 38.34(4) . . ?
O4 C1 O2 119.4(2) . . ?
O4 C1 O1 118.3(2) . . ?
O2 C1 O1 122.27(19) . . ?
C1 O1 Ru1 120.00(14) . 3_655 ?
C1 O2 Ru1 120.70(14) . . ?
Ru1 O3 Ru1 78.18(6) . 3_655 ?
Ru1 O5 Mg1 102.26(7) . . ?
Ru1 O5 H1 112(2) . . ?
Mg1 O5 H1 114(2) . . ?
Ru1 O6 Mg1 101.90(7) . . ?
Ru1 O6 H2 113(2) . . ?
Mg1 O6 H2 102(2) . . ?
Mg1 O7 H3 121(2) . . ?
Mg1 O7 H4 120(2) . . ?
H3 O7 H4 102(3) . . ?
Mg1 O8 H5 127(2) . . ?
Mg1 O8 H6 113(3) . . ?
H5 O8 H6 112(3) . . ?
Mg1 O9 H7 128(2) . . ?
Mg1 O9 H8 122(3) . . ?
H7 O9 H8 110(4) . . ?
Mg1 O10 H9 124(3) . . ?
Mg1 O10 H10 133(3) . . ?
H9 O10 H10 104(4) . . ?
H11 O11 H12 104(4) . . ?
H13 O12 H14 106(4) . . ?

_refine_diff_density_max         0.513
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.087

####################################################################### 
# 
# 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_p21n
_database_code_depnum_ccdc_archive 'CCDC 2308506'
loop_
_audit_author_name
_audit_author_address
'Bin Liu'
;Northwest University
China
;
_audit_update_record             
;
2024-01-11 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT305_p21n                
;
PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??) H7B Check 
RESPONSE: ...
;
_vrf_PLAT415_p21n                
;
PROBLEM: Short Inter D-H..H-X H7C ..H7D . 1.67 Ang. 
RESPONSE: disordered C7 (CH3 group) resulted the Alert level A  problem
;
_vrf_PLAT213_p21n                
;
PROBLEM: Atom C7 has ADP max/min Ratio ..... 4.1 oblate
RESPONSE: disordered C7 (CH3 group) resulted the Alert level B  problem
;
_vrf_PLAT234_p21n                
;
PROBLEM: Large Hirshfeld Difference C5 --C7 . 0.30 Ang. 
RESPONSE: disordered C7 (CH3 group) resulted the Alert level B  problem
;
_vrf_PLAT260_p21n                
;
PROBLEM: Large Average Ueq of Residue Including O7 0.385 Check 
RESPONSE: disordered lattice water O7 resulted the Alert level B  problem
;
_vrf_PLAT420_p21n                
;
PROBLEM: D-H Bond Without Acceptor O7 --H7A . Please Check 
RESPONSE: disordered lattice water O7 resulted the Alert level B  problem
;
# end Validation Reply Form
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H24 N4 O10 Ru2, 4(H2 O), 2(H2 O)'
_chemical_formula_sum            'C12 H36 N4 O14 Ru2'
_chemical_formula_weight         662.59

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.1532(3)
_cell_length_b                   13.3890(5)
_cell_length_c                   11.9650(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.039(2)
_cell_angle_gamma                90
_cell_volume                     1145.94(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3593
_cell_measurement_theta_min      5.75
_cell_measurement_theta_max      54.75

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_F_000             672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.392
_shelx_estimated_absorpt_T_min   0.851
_shelx_estimated_absorpt_T_max   0.934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7170
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.043
_diffrn_reflns_theta_max         25.644
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             2125
_reflns_number_gt                1745
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0616P)²+3.6086P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2125
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1173
_refine_ls_wR_factor_gt          0.1111
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.37858(6) 0.53724(3) 0.05373(3) 0.01452(19) Uani 1 1 d . . . . .
N1 N 0.3381(7) 0.6684(3) 0.1548(4) 0.0240(11) Uani 1 1 d . . . . .
H1A H 0.213745 0.677836 0.158882 0.029 Uiso 1 1 d R U . . .
N2 N 0.4374(7) 0.8400(3) 0.2890(4) 0.0293(12) Uani 1 1 d . . . . .
H2A H 0.405947 0.893860 0.329918 0.035 Uiso 1 1 d R U . . .
H2B H 0.562697 0.834480 0.286958 0.035 Uiso 1 1 d R U . . .
C1 C 0.6112(8) 0.3961(4) 0.1780(5) 0.0244(13) Uani 1 1 d . . . . .
C2 C 0.4151(9) 0.7611(4) 0.1046(5) 0.0281(14) Uani 1 1 d . . . . .
H2C H 0.367114 0.768847 0.030177 0.034 Uiso 1 1 d R U . . .
H2D H 0.548683 0.755756 0.100057 0.034 Uiso 1 1 d R U . . .
C3 C 0.4036(9) 0.6576(4) 0.2708(5) 0.0297(14) Uani 1 1 d . . . . .
H3A H 0.536575 0.647789 0.270417 0.036 Uiso 1 1 d R U . . .
H3B H 0.347255 0.599539 0.303707 0.036 Uiso 1 1 d R U . . .
C4 C 0.3592(10) 0.7494(4) 0.3436(5) 0.0338(15) Uani 1 1 d . . . . .
H4A H 0.225785 0.756400 0.347539 0.041 Uiso 1 1 d R U . . .
C5 C 0.3639(10) 0.8527(4) 0.1736(5) 0.0320(15) Uani 1 1 d . . . . .
H5E H 0.230414 0.859848 0.175738 0.038 Uiso 1 1 d R U . . .
C6 C 0.4277(14) 0.7369(7) 0.4590(8) 0.033(2) Uani 0.6456 1 d . . P . .
H6C H 0.560922 0.728612 0.456342 0.040 Uiso 1 1 d R U . . .
H6A H 0.397242 0.794902 0.502421 0.050 Uiso 1 1 d R U . . .
H6B H 0.371512 0.678972 0.492352 0.050 Uiso 1 1 d R U . . .
O1 O 0.3755(5) 0.4174(2) -0.0348(3) 0.0213(8) Uani 1 1 d . . . . .
O2 O 0.4664(6) 0.4538(3) 0.1874(3) 0.0225(9) Uani 1 1 d . . . . .
O3 O 0.7021(5) 0.3838(3) 0.0843(3) 0.0215(8) Uani 1 1 d . . . . .
O4 O 0.6709(6) 0.3498(3) 0.2630(4) 0.0371(11) Uani 1 1 d . . . . .
O5 O 0.1103(6) 0.5073(3) 0.0949(3) 0.0270(9) Uani 1 1 d . . . . .
H5C H 0.041123 0.554606 0.071824 0.032 Uiso 1 1 d R U . . .
O6 O 0.5696(10) 0.1480(6) 0.2600(10) 0.150(5) Uani 1 1 d . . . . .
H6G H 0.600697 0.209268 0.260192 0.225 Uiso 1 1 d R U . . .
H6E H 0.641217 0.115618 0.303672 0.225 Uiso 1 1 d R U . . .
O7 O 0.702(4) 0.4936(14) 0.4379(10) 0.385(18) Uani 1 1 d . . . . .
H7D H 0.698343 0.450648 0.385611 0.462 Uiso 1 1 d R U . . .
H7A H 0.738633 0.549460 0.412151 0.577 Uiso 1 1 d R U . . .
C7 C 0.438(4) 0.9384(19) 0.122(3) 0.077(10) Uani 0.3086 1 d . . P . .
H7B H 0.407875 0.997437 0.163990 0.115 Uiso 1 1 d R U . . .
H7C H 0.571116 0.930497 0.119000 0.115 Uiso 1 1 d R U . . .
H7E H 0.389116 0.944526 0.047640 0.115 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 O1 1.875(4) 3_665 ?
Ru1 O1 1.923(3) . ?
Ru1 O5 2.022(4) . ?
Ru1 O3 2.044(3) 3_665 ?
Ru1 O2 2.049(4) . ?
Ru1 N1 2.151(4) . ?
Ru1 Ru1 2.3808(9) 3_665 ?
N1 C3 1.472(7) . ?
N1 C2 1.485(7) . ?
N1 H1A 0.9001 . ?
N2 C5 1.486(8) . ?
N2 C4 1.488(8) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
C1 O4 1.265(7) . ?
C1 O2 1.297(7) . ?
C1 O3 1.307(7) . ?
C2 C5 1.523(8) . ?
C2 H2C 0.9599 . ?
C2 H2D 0.9600 . ?
C3 C4 1.540(8) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C4 C6 1.474(11) . ?
C4 H4A 0.9600 . ?
C5 C7 1.41(3) . ?
C5 H5E 0.9600 . ?
C6 H6C 0.9600 . ?
C6 H6A 0.9598 . ?
C6 H6B 0.9602 . ?
O5 H5C 0.8500 . ?
O6 H6G 0.8499 . ?
O6 H6E 0.8501 . ?
O7 H7D 0.8500 . ?
O7 H7A 0.8501 . ?
C7 H7B 0.9599 . ?
C7 H7C 0.9599 . ?
C7 H7E 0.9600 . ?

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 102.38(13) 3_665 . ?
O1 Ru1 O5 169.89(15) 3_665 . ?
O1 Ru1 O5 87.61(16) . . ?
O1 Ru1 O3 89.96(15) 3_665 3_665 ?
O1 Ru1 O3 89.04(15) . 3_665 ?
O5 Ru1 O3 91.84(15) . 3_665 ?
O1 Ru1 O2 89.08(16) 3_665 . ?
O1 Ru1 O2 88.74(15) . . ?
O5 Ru1 O2 89.54(16) . . ?
O3 Ru1 O2 177.33(15) 3_665 . ?
O1 Ru1 N1 85.97(17) 3_665 . ?
O1 Ru1 N1 171.55(17) . . ?
O5 Ru1 N1 84.09(17) . . ?
O3 Ru1 N1 89.67(16) 3_665 . ?
O2 Ru1 N1 92.74(16) . . ?
O1 Ru1 Ru1 52.10(11) 3_665 3_665 ?
O1 Ru1 Ru1 50.28(12) . 3_665 ?
O5 Ru1 Ru1 137.86(11) . 3_665 ?
O3 Ru1 Ru1 89.19(11) 3_665 3_665 ?
O2 Ru1 Ru1 88.26(12) . 3_665 ?
N1 Ru1 Ru1 138.06(14) . 3_665 ?
C3 N1 C2 110.2(4) . . ?
C3 N1 Ru1 114.0(3) . . ?
C2 N1 Ru1 113.9(4) . . ?
C3 N1 H1A 106.0 . . ?
C2 N1 H1A 105.7 . . ?
Ru1 N1 H1A 106.2 . . ?
C5 N2 C4 111.6(4) . . ?
C5 N2 H2A 109.0 . . ?
C4 N2 H2A 108.7 . . ?
C5 N2 H2B 109.6 . . ?
C4 N2 H2B 108.6 . . ?
H2A N2 H2B 109.3 . . ?
O4 C1 O2 119.5(5) . . ?
O4 C1 O3 117.4(5) . . ?
O2 C1 O3 123.1(5) . . ?
N1 C2 C5 111.4(5) . . ?
N1 C2 H2C 109.4 . . ?
C5 C2 H2C 109.3 . . ?
N1 C2 H2D 109.3 . . ?
C5 C2 H2D 109.3 . . ?
H2C C2 H2D 108.1 . . ?
N1 C3 C4 112.9(5) . . ?
N1 C3 H3A 108.9 . . ?
C4 C3 H3A 108.5 . . ?
N1 C3 H3B 109.4 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C6 C4 N2 112.3(6) . . ?
C6 C4 C3 111.8(6) . . ?
N2 C4 C3 109.0(5) . . ?
C6 C4 H4A 107.2 . . ?
N2 C4 H4A 108.4 . . ?
C3 C4 H4A 108.2 . . ?
C7 C5 N2 111.6(14) . . ?
C7 C5 C2 109.2(11) . . ?
N2 C5 C2 109.0(5) . . ?
C7 C5 H5E 107.8 . . ?
N2 C5 H5E 109.7 . . ?
C2 C5 H5E 109.5 . . ?
C4 C6 H6C 108.2 . . ?
C4 C6 H6A 109.9 . . ?
H6C C6 H6A 109.7 . . ?
C4 C6 H6B 110.0 . . ?
H6C C6 H6B 109.7 . . ?
H6A C6 H6B 109.5 . . ?
Ru1 O1 Ru1 77.62(13) 3_665 . ?
C1 O2 Ru1 120.1(4) . . ?
C1 O3 Ru1 119.2(3) . 3_665 ?
Ru1 O5 H5C 109.0 . . ?
H6G O6 H6E 109.5 . . ?
H7D O7 H7A 109.8 . . ?
C5 C7 H7B 111.0 . . ?
C5 C7 H7C 107.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C7 H7E 109.9 . . ?
H7B C7 H7E 109.5 . . ?
H7C C7 H7E 109.5 . . ?

_refine_diff_density_max         1.724
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.161

