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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_kru216
_database_code_depnum_ccdc_archive 'CCDC 1979798'
loop_
_audit_author_name
_audit_author_address
'Kuratieva N.V.'
;Nikolaev Institute of Inorganic Chemistry
Russia
;
_audit_update_record             
;
2020-01-24 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'H N5 O10 Ru, H12 N4 Pd'
_chemical_formula_sum            'H13 N9 O10 Pd Ru'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      298(2)
_chemical_formula_weight         506.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   7.8002(3)
_cell_length_b                   7.8688(3)
_cell_length_c                   11.9165(5)
_cell_angle_alpha                106.3890(10)
_cell_angle_beta                 91.0570(10)
_cell_angle_gamma                93.1170(10)
_cell_volume                     700.22(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2405
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      27.53
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.403
_exptl_crystal_F_000             492
_exptl_transmission_factor_min   0.659
_exptl_transmission_factor_max   0.746
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.431
_shelx_estimated_absorpt_T_min   0.605
_shelx_estimated_absorpt_T_max   0.811

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?


_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex DUO CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_reflns_number            6347
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.782
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_full        25.250
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3226
_reflns_number_gt                2430
_reflns_threshold_expression     >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    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0208P)²+0.5348P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3226
_refine_ls_number_parameters     192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0243
_refine_ls_wR_factor_ref         0.0645
_refine_ls_wR_factor_gt          0.0598
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
Pd2 Pd 0.0000 0.0000 0.5000 0.01984(8) Uani 1 2 d S . P . .
Pd1 Pd 0.0000 0.0000 0.0000 0.02176(8) Uani 1 2 d S . P . .
Ru3 Ru 0.49479(2) 0.49647(2) 0.24996(2) 0.01908(7) Uani 1 1 d . . . . .
O1 O 0.4833(3) 0.3130(2) 0.10195(17) 0.0293(4) Uani 1 1 d . . . . .
H1 H 0.4902 0.3589 0.0482 0.035 Uiso 1 1 calc R U . . .
N32 N 0.6952(3) 0.6331(3) 0.1897(2) 0.0263(5) Uani 1 1 d . . . . .
N31 N 0.3198(3) 0.6339(3) 0.1790(2) 0.0281(5) Uani 1 1 d . . . . .
N35 N 0.5010(3) 0.6687(3) 0.3824(2) 0.0326(5) Uani 1 1 d . . . . .
N34 N 0.2959(3) 0.3440(3) 0.2972(2) 0.0282(5) Uani 1 1 d . . . . .
N33 N 0.6722(3) 0.3529(3) 0.3132(2) 0.0322(6) Uani 1 1 d . . . . .
N22 N -0.0045(3) 0.2694(3) 0.5425(2) 0.0318(5) Uani 1 1 d . . . . .
H22A H 0.0983 0.3157 0.5313 0.048 Uiso 1 1 calc R U . . .
H22B H -0.0305 0.3114 0.6172 0.048 Uiso 1 1 calc R U . . .
H22C H -0.0832 0.2988 0.4974 0.048 Uiso 1 1 calc R U . . .
O311 O 0.2894(3) 0.5949(3) 0.0721(2) 0.0434(6) Uani 1 1 d . . . . .
N11 N 0.0297(3) 0.2683(3) 0.0333(2) 0.0353(6) Uani 1 1 d . . . . .
H11A H 0.0017 0.3198 0.1066 0.053 Uiso 1 1 calc R U . . .
H11B H -0.0382 0.3031 -0.0158 0.053 Uiso 1 1 calc R U . . .
H11C H 0.1387 0.2995 0.0237 0.053 Uiso 1 1 calc R U . . .
O332 O 0.7254(3) 0.4118(3) 0.4162(2) 0.0534(7) Uani 1 1 d . . . . .
O321 O 0.8452(3) 0.5924(3) 0.1947(2) 0.0470(6) Uani 1 1 d . . . . .
O312 O 0.2495(3) 0.7579(3) 0.2432(2) 0.0609(8) Uani 1 1 d . . . . .
O322 O 0.6658(3) 0.7591(3) 0.1528(3) 0.0568(7) Uani 1 1 d . . . . .
O331 O 0.7249(4) 0.2157(3) 0.2524(2) 0.0678(9) Uani 1 1 d . . . . .
O342 O 0.1532(3) 0.3956(4) 0.3153(3) 0.0798(7) Uani 1 1 d . . . . .
N21 N -0.0176(3) -0.0031(3) 0.3281(2) 0.0273(5) Uani 1 1 d . . . . .
H21A H 0.0787 0.0465 0.3092 0.041 Uiso 1 1 calc R U . . .
H21B H -0.1063 0.0575 0.3170 0.041 Uiso 1 1 calc R U . . .
H21C H -0.0329 -0.1147 0.2834 0.041 Uiso 1 1 calc R U . . .
N12 N 0.2593(3) -0.0199(3) 0.0159(2) 0.0361(6) Uani 1 1 d . . . . .
H12A H 0.3117 0.0882 0.0377 0.054 Uiso 1 1 calc R U . . .
H12B H 0.2981 -0.0809 -0.0526 0.054 Uiso 1 1 calc R U . . .
H12C H 0.2809 -0.0757 0.0696 0.054 Uiso 1 1 calc R U . . .
O341 O 0.3185(3) 0.1934(3) 0.2978(3) 0.0798(7) Uani 1 1 d . . . . .
O351 O 0.5061(4) 0.7915(3) 0.4607(2) 0.0752(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd2 N22 2.039(2) 2_556 ?
Pd2 N22 2.039(2) . ?
Pd2 N21 2.043(2) . ?
Pd2 N21 2.043(2) 2_556 ?
Pd1 N11 2.035(2) . ?
Pd1 N11 2.035(2) 2 ?
Pd1 N12 2.047(2) 2 ?
Pd1 N12 2.047(2) . ?
Ru3 N35 1.764(2) . ?
Ru3 O1 1.9355(18) . ?
Ru3 N33 2.091(2) . ?
Ru3 N34 2.092(2) . ?
Ru3 N31 2.093(2) . ?
Ru3 N32 2.100(2) . ?
O1 H1 0.8200 . ?
N32 O322 1.223(3) . ?
N32 O321 1.235(3) . ?
N31 O312 1.222(3) . ?
N31 O311 1.238(3) . ?
N35 O351 1.137(3) . ?
N34 O342 1.207(3) . ?
N34 O341 1.209(3) . ?
N33 O331 1.216(3) . ?
N33 O332 1.238(3) . ?
N22 H22A 0.8900 . ?
N22 H22B 0.8900 . ?
N22 H22C 0.8900 . ?
N11 H11A 0.8900 . ?
N11 H11B 0.8900 . ?
N11 H11C 0.8900 . ?
N21 H21A 0.8900 . ?
N21 H21B 0.8900 . ?
N21 H21C 0.8900 . ?
N12 H12A 0.8900 . ?
N12 H12B 0.8900 . ?
N12 H12C 0.8900 . ?

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
N22 Pd2 N22 180.0 2_556 . ?
N22 Pd2 N21 92.22(9) 2_556 . ?
N22 Pd2 N21 87.78(9) . . ?
N22 Pd2 N21 87.78(9) 2_556 2_556 ?
N22 Pd2 N21 92.22(9) . 2_556 ?
N21 Pd2 N21 180.0 . 2_556 ?
N11 Pd1 N11 180.0 . 2 ?
N11 Pd1 N12 88.24(9) . 2 ?
N11 Pd1 N12 91.76(9) 2 2 ?
N11 Pd1 N12 91.76(9) . . ?
N11 Pd1 N12 88.24(9) 2 . ?
N12 Pd1 N12 180.0 2 . ?
N35 Ru3 O1 177.88(9) . . ?
N35 Ru3 N33 93.09(11) . . ?
O1 Ru3 N33 88.99(9) . . ?
N35 Ru3 N34 95.13(10) . . ?
O1 Ru3 N34 85.29(9) . . ?
N33 Ru3 N34 89.10(9) . . ?
N35 Ru3 N31 89.32(11) . . ?
O1 Ru3 N31 88.59(9) . . ?
N33 Ru3 N31 177.42(9) . . ?
N34 Ru3 N31 91.60(9) . . ?
N35 Ru3 N32 89.52(10) . . ?
O1 Ru3 N32 90.06(9) . . ?
N33 Ru3 N32 90.49(9) . . ?
N34 Ru3 N32 175.34(8) . . ?
N31 Ru3 N32 88.62(9) . . ?
Ru3 O1 H1 109.5 . . ?
O322 N32 O321 118.7(2) . . ?
O322 N32 Ru3 120.30(18) . . ?
O321 N32 Ru3 120.90(18) . . ?
O312 N31 O311 119.0(2) . . ?
O312 N31 Ru3 119.8(2) . . ?
O311 N31 Ru3 121.16(17) . . ?
O351 N35 Ru3 172.8(3) . . ?
O342 N34 O341 117.8(3) . . ?
O342 N34 Ru3 122.26(19) . . ?
O341 N34 Ru3 119.66(19) . . ?
O331 N33 O332 119.5(2) . . ?
O331 N33 Ru3 122.4(2) . . ?
O332 N33 Ru3 118.17(19) . . ?
Pd2 N22 H22A 109.5 . . ?
Pd2 N22 H22B 109.5 . . ?
H22A N22 H22B 109.5 . . ?
Pd2 N22 H22C 109.5 . . ?
H22A N22 H22C 109.5 . . ?
H22B N22 H22C 109.5 . . ?
Pd1 N11 H11A 109.5 . . ?
Pd1 N11 H11B 109.5 . . ?
H11A N11 H11B 109.5 . . ?
Pd1 N11 H11C 109.5 . . ?
H11A N11 H11C 109.5 . . ?
H11B N11 H11C 109.5 . . ?
Pd2 N21 H21A 109.5 . . ?
Pd2 N21 H21B 109.5 . . ?
H21A N21 H21B 109.5 . . ?
Pd2 N21 H21C 109.5 . . ?
H21A N21 H21C 109.5 . . ?
H21B N21 H21C 109.5 . . ?
Pd1 N12 H12A 109.5 . . ?
Pd1 N12 H12B 109.5 . . ?
H12A N12 H12B 109.5 . . ?
Pd1 N12 H12C 109.5 . . ?
H12A N12 H12C 109.5 . . ?
H12B N12 H12C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O311 0.82 2.45 2.850(3) 110.9 .
O1 H1 O311 0.82 2.34 2.969(3) 134.4 2_665
O1 H1 O322 0.82 2.57 3.117(3) 125.6 2_665
N22 H22A O332 0.89 2.40 3.153(3) 142.2 2_666
N22 H22B O321 0.89 2.55 3.213(4) 132.1 2_666
N22 H22B O312 0.89 2.55 3.266(4) 138.1 2_566
N22 H22B O342 0.89 2.47 3.008(4) 119.4 2_566
N22 H22C O332 0.89 2.13 3.008(3) 169.4 1_455
N11 H11A O321 0.89 2.50 3.163(3) 131.7 1_455
N11 H11A O342 0.89 2.63 3.332(5) 136.4 .
N11 H11B O311 0.89 2.32 3.142(3) 154.4 2_565
N11 H11C O311 0.89 2.46 3.106(3) 130.1 .
N11 H11C O322 0.89 2.57 3.253(4) 134.1 2_665
N21 H21A O341 0.89 2.17 3.050(3) 169.2 .
N21 H21B O331 0.89 2.13 3.000(3) 163.9 1_455
N21 H21C O321 0.89 2.38 3.243(3) 162.3 1_445
N21 H21C O312 0.89 2.47 2.886(3) 109.2 1_545
N12 H12A O1 0.89 2.11 2.981(3) 166.4 .
N12 H12B O1 0.89 2.52 3.178(3) 131.1 2_655
N12 H12B O331 0.89 2.32 3.141(4) 154.1 2_655
N12 H12C O311 0.89 2.61 3.303(3) 135.9 1_545
O1 H1 O311 0.82 2.45 2.850(3) 110.9 .
O1 H1 O311 0.82 2.34 2.969(3) 134.4 2_665
O1 H1 O322 0.82 2.57 3.117(3) 125.6 2_665
N22 H22A O332 0.89 2.40 3.153(3) 142.2 2_666
N22 H22B O321 0.89 2.55 3.213(4) 132.1 2_666
N22 H22B O312 0.89 2.55 3.266(4) 138.1 2_566
N22 H22B O342 0.89 2.47 3.008(4) 119.4 2_566
N22 H22C O332 0.89 2.13 3.008(3) 169.4 1_455
N11 H11A O321 0.89 2.50 3.163(3) 131.7 1_455
N11 H11A O342 0.89 2.63 3.332(5) 136.4 .
N11 H11B O311 0.89 2.32 3.142(3) 154.4 2_565
N11 H11C O311 0.89 2.46 3.106(3) 130.1 .
N11 H11C O322 0.89 2.57 3.253(4) 134.1 2_665
N21 H21A O341 0.89 2.17 3.050(3) 169.2 .
N21 H21B O331 0.89 2.13 3.000(3) 163.9 1_455
N21 H21C O321 0.89 2.38 3.243(3) 162.3 1_445
N12 H12A O1 0.89 2.11 2.981(3) 166.4 .
N12 H12B O1 0.89 2.52 3.178(3) 131.1 2_655
N12 H12B O331 0.89 2.32 3.141(4) 154.1 2_655
N12 H12C O311 0.89 2.61 3.303(3) 135.9 1_545

_refine_diff_density_max         0.881
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.086


_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_symmetry_cell_setting           ?
_symmetry_space_group_name_h-m   ?
_symmetry_int_tables_number      ?
_chemical_absolute_configuration ?

####################################################################### 
# 
# 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_kru217m
_database_code_depnum_ccdc_archive 'CCDC 1979799'
loop_
_audit_author_name
_audit_author_address
'Kuratieva N.V.'
;Nikolaev Institute of Inorganic Chemistry
Russia
;
_audit_update_record             
;
2020-01-24 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'H13 N9 O10 Pd Ru'
_chemical_formula_sum            'H13 N9 O10 Pd Ru'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      383(2)
_chemical_formula_weight         506.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           10
_space_group_name_H-M_alt        'P 2/m'
_space_group_name_Hall           '-P 2y'

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

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

_cell_length_a                   7.851(2)
_cell_length_b                   7.792(2)
_cell_length_c                   12.456(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.148(7)
_cell_angle_gamma                90
_cell_volume                     735.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    383(2)
_cell_measurement_reflns_used    2355
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      27.47
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_F_000             492
_exptl_transmission_factor_min   0.654
_exptl_transmission_factor_max   0.786
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.314
_shelx_estimated_absorpt_T_min   0.595
_shelx_estimated_absorpt_T_max   0.934

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?


_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Apex DUO CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_reflns_number            6160
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.694
_diffrn_reflns_theta_max         27.833
_diffrn_reflns_theta_full        25.250
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1837
_reflns_number_gt                1333
_reflns_threshold_expression     >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    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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)+(0.0156P)²+2.5446P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1837
_refine_ls_number_parameters     129
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1048
_refine_ls_wR_factor_gt          0.0977
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.197
_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
Pd1 Pd 0.0000 0.0000 0.5000 0.0341(2) Uani 1 4 d S T P . .
Pd2 Pd 0.0000 0.0000 0.0000 0.0372(2) Uani 1 4 d S T P . .
Ru3 Ru 0.51206(7) 0.5000 0.25282(5) 0.03193(18) Uani 1 2 d S T P A .
O1 O 0.6835(8) 0.5000 0.3951(5) 0.066(3) Uani 1 2 d S T P . .
H1 H 0.6398 0.5426 0.4419 0.079 Uiso 0.5 1 calc R U P . .
N34 N 0.3721(8) 0.3139(9) 0.3133(5) 0.0538(14) Uani 1 1 d . . . . .
N33 N 0.6616(7) 0.3129(10) 0.2022(5) 0.0557(16) Uani 1 1 d . . . . .
N35 N 0.3521(11) 0.5000 0.1244(6) 0.056(2) Uani 1 2 d S T P . .
O351 O 0.2374(13) 0.5000 0.0475(7) 0.120(5) Uani 1 2 d S T P A .
N11 N -0.2688(10) 0.0000 0.4738(8) 0.071(3) Uani 1 2 d S T P . .
H11A H -0.3125 0.0990 0.4429 0.107 Uiso 0.5 1 calc R U P . .
H11B H -0.2957 -0.0129 0.5385 0.107 Uiso 0.5 1 calc R U P . .
H11C H -0.3150 -0.0861 0.4286 0.107 Uiso 0.5 1 calc R U P . .
N22 N 0.2691(10) 0.0000 0.0431(7) 0.053(2) Uani 1 2 d S T P . .
H22A H 0.3090 -0.0262 0.1149 0.080 Uiso 0.5 1 calc R U P . .
H22B H 0.3080 0.1036 0.0309 0.080 Uiso 0.5 1 calc R U P . .
H22C H 0.3077 -0.0774 0.0025 0.080 Uiso 0.5 1 calc R U P . .
N21 N -0.0041(11) 0.0000 0.1627(6) 0.058(2) Uani 1 2 d S T P . .
H21A H -0.0944 0.0632 0.1708 0.087 Uiso 0.5 1 calc R U P . .
H21B H 0.0964 0.0439 0.2040 0.087 Uiso 0.5 1 calc R U P . .
H21C H -0.0161 -0.1071 0.1844 0.087 Uiso 0.5 1 calc R U P . .
N12 N 0.0000 -0.2539(13) 0.5000 0.078(3) Uani 1 2 d S T P . .
H12A H 0.1105 -0.2920 0.5140 0.116 Uiso 0.5 1 calc R U P . .
H12B H -0.0613 -0.2920 0.4338 0.116 Uiso 0.5 1 calc R U P . .
H12C H -0.0492 -0.2920 0.5522 0.116 Uiso 0.5 1 calc R U P . .
O342 O 0.399(2) 0.283(2) 0.4123(11) 0.113(5) Uani 0.597(18) 1 d . . P A 2
O341 O 0.250(2) 0.247(2) 0.2529(10) 0.113(5) Uani 0.597(18) 1 d . U P A 2
O332 O 0.5951(15) 0.226(2) 0.1202(13) 0.099(4) Uani 0.63(3) 1 d . . P A 1
O331 O 0.8212(15) 0.303(3) 0.2462(11) 0.099(4) Uani 0.63(3) 1 d . U P A 1
O343 O 0.386(3) 0.161(3) 0.2957(17) 0.100(6) Uani 0.403(18) 1 d . U P A 1
O344 O 0.267(3) 0.346(3) 0.3620(16) 0.100(6) Uani 0.403(18) 1 d . . P A 1
O333 O 0.748(4) 0.201(4) 0.2646(16) 0.103(7) Uani 0.37(3) 1 d . U P A 2
O334 O 0.660(4) 0.283(4) 0.113(2) 0.103(7) Uani 0.37(3) 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N12 1.978(10) . ?
Pd1 N12 1.978(10) 3_556 ?
Pd1 N11 2.049(7) . ?
Pd1 N11 2.049(7) 3_556 ?
Pd2 N21 2.035(7) . ?
Pd2 N21 2.035(7) 3 ?
Pd2 N22 2.039(8) . ?
Pd2 N22 2.039(8) 3 ?
Ru3 N35 1.757(8) . ?
Ru3 O1 1.925(6) . ?
Ru3 N33 2.071(6) . ?
Ru3 N33 2.071(6) 4_565 ?
Ru3 N34 2.076(6) 4_565 ?
Ru3 N34 2.076(6) . ?
O1 H1 0.8200 . ?
N34 O344 1.173(17) . ?
N34 O341 1.174(14) . ?
N34 O342 1.219(13) . ?
N34 O343 1.22(2) . ?
N33 O334 1.14(2) . ?
N33 O332 1.225(14) . ?
N33 O331 1.232(11) . ?
N33 O333 1.24(2) . ?
N35 O351 1.131(11) . ?
N11 H11A 0.8900 . ?
N11 H11B 0.8900 . ?
N11 H11C 0.8900 . ?
N22 H22A 0.8900 . ?
N22 H22B 0.8900 . ?
N22 H22C 0.8900 . ?
N21 H21A 0.8900 . ?
N21 H21B 0.8900 . ?
N21 H21C 0.8900 . ?
N12 H12A 0.8900 . ?
N12 H12B 0.8900 . ?
N12 H12C 0.8900 . ?

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
N12 Pd1 N12 180.0 . 3_556 ?
N12 Pd1 N11 90.000(2) . . ?
N12 Pd1 N11 90.000(1) 3_556 . ?
N12 Pd1 N11 90.000(1) . 3_556 ?
N12 Pd1 N11 90.000(2) 3_556 3_556 ?
N11 Pd1 N11 180.0 . 3_556 ?
N21 Pd2 N21 180.0 . 3 ?
N21 Pd2 N22 91.3(3) . . ?
N21 Pd2 N22 88.7(3) 3 . ?
N21 Pd2 N22 88.7(3) . 3 ?
N21 Pd2 N22 91.3(3) 3 3 ?
N22 Pd2 N22 180.0 . 3 ?
N35 Ru3 O1 178.8(3) . . ?
N35 Ru3 N33 92.9(2) . . ?
O1 Ru3 N33 88.0(2) . . ?
N35 Ru3 N33 92.9(2) . 4_565 ?
O1 Ru3 N33 88.0(2) . 4_565 ?
N33 Ru3 N33 89.5(4) . 4_565 ?
N35 Ru3 N34 90.6(3) . 4_565 ?
O1 Ru3 N34 88.6(2) . 4_565 ?
N33 Ru3 N34 176.5(2) . 4_565 ?
N33 Ru3 N34 90.8(3) 4_565 4_565 ?
N35 Ru3 N34 90.6(3) . . ?
O1 Ru3 N34 88.6(2) . . ?
N33 Ru3 N34 90.8(3) . . ?
N33 Ru3 N34 176.5(2) 4_565 . ?
N34 Ru3 N34 88.6(4) 4_565 . ?
Ru3 O1 H1 109.5 . . ?
O341 N34 O342 117.3(10) . . ?
O344 N34 O343 114.3(14) . . ?
O344 N34 Ru3 123.3(11) . . ?
O341 N34 Ru3 119.8(8) . . ?
O342 N34 Ru3 122.4(7) . . ?
O343 N34 Ru3 122.3(9) . . ?
O332 N33 O331 119.9(9) . . ?
O334 N33 O333 109.5(16) . . ?
O334 N33 Ru3 125.5(13) . . ?
O332 N33 Ru3 119.5(6) . . ?
O331 N33 Ru3 120.0(8) . . ?
O333 N33 Ru3 124.3(9) . . ?
O351 N35 Ru3 173.4(9) . . ?
Pd1 N11 H11A 109.5 . . ?
Pd1 N11 H11B 109.5 . . ?
H11A N11 H11B 109.5 . . ?
Pd1 N11 H11C 109.5 . . ?
H11A N11 H11C 109.5 . . ?
H11B N11 H11C 109.5 . . ?
Pd2 N22 H22A 109.5 . . ?
Pd2 N22 H22B 109.5 . . ?
H22A N22 H22B 109.5 . . ?
Pd2 N22 H22C 109.5 . . ?
H22A N22 H22C 109.5 . . ?
H22B N22 H22C 109.5 . . ?
Pd2 N21 H21A 109.5 . . ?
Pd2 N21 H21B 109.5 . . ?
H21A N21 H21B 109.5 . . ?
Pd2 N21 H21C 109.5 . . ?
H21A N21 H21C 109.5 . . ?
H21B N21 H21C 109.5 . . ?
Pd1 N12 H12A 109.5 . . ?
Pd1 N12 H12B 109.5 . . ?
H12A N12 H12B 109.5 . . ?
Pd1 N12 H12C 109.5 . . ?
H12A N12 H12C 109.5 . . ?
H12B N12 H12C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O342 0.82 2.35 3.139(16) 161.2 3_666
O1 H1 O342 0.82 2.28 2.852(13) 127.5 4_565
O1 H1 O344 0.82 2.51 3.18(2) 139.5 3_666
N11 H11A O342 0.89 2.62 3.35(2) 139.3 1_455
N11 H11A O342 0.89 2.53 2.947(15) 109.2 2_556
N11 H11B O342 0.89 2.39 2.947(15) 120.5 3_556
N11 H11B O343 0.89 2.62 3.470(18) 160.1 3_556
N11 H11C O343 0.89 2.56 3.27(3) 137.2 4_455
N11 H11C O333 0.89 2.40 3.08(3) 132.8 4_455
N22 H22A O341 0.89 2.56 3.280(16) 138.7 4
N22 H22A O343 0.89 2.41 3.29(2) 166.7 4
N22 H22B O332 0.89 2.43 3.046(16) 126.5 .
N22 H22B O332 0.89 2.40 3.082(15) 133.3 2_655
N22 H22B O334 0.89 2.34 3.08(3) 141.7 2_655
N22 H22C O332 0.89 2.20 3.082(15) 168.6 3_655
N22 H22C O334 0.89 2.21 3.08(3) 167.0 3_655
N21 H21A O332 0.89 2.67 3.521(13) 160.0 1_455
N21 H21A O331 0.89 2.27 3.048(13) 146.2 1_455
N21 H21A O333 0.89 2.19 3.02(2) 155.3 1_455
N21 H21A O334 0.89 2.54 3.37(2) 155.3 1_455
N21 H21B O341 0.89 1.99 2.789(14) 149.2 .
N21 H21B O343 0.89 2.44 3.32(2) 172.5 .
N21 H21C O341 0.89 2.31 2.789(14) 113.4 4
N21 H21C O331 0.89 2.25 3.048(13) 148.7 4_455
N21 H21C O333 0.89 2.43 3.02(2) 124.1 4_455
N12 H12A O1 0.89 2.36 3.141(8) 146.5 3_656
N12 H12A O333 0.89 2.78 3.10(2) 102.9 3_656
N12 H12B O1 0.89 2.52 3.141(8) 127.0 1_445
N12 H12B O331 0.89 2.28 3.130(14) 159.9 4_455
N12 H12B O333 0.89 2.35 3.10(2) 142.5 4_455
N12 H12C O344 0.89 2.28 3.121(15) 157.9 3_556

_refine_diff_density_max         0.891
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.115


_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_symmetry_cell_setting           ?
_symmetry_space_group_name_h-m   ?
_symmetry_int_tables_number      ?
_chemical_absolute_configuration ?

