# Electronic Supplementary Material (ESI) for ChemComm.
# 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_xb0484
_database_code_depnum_ccdc_archive 'CCDC 1901103'
loop_
_audit_author_name
_audit_author_address
'Bin Liu' 'Northwest University'
_audit_update_record             
;
2019-03-07 deposited with the CCDC.	2019-12-16 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         'C4 H8 Na Ni O16 Ru2, 3(H2O)'
_chemical_formula_sum            'C4 H14 Na Ni O19 Ru2'
_chemical_formula_weight         649.99

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'
O O 0.0106 0.0060 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

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

_cell_length_a                   18.251(3)
_cell_length_b                   9.2828(16)
_cell_length_c                   10.1645(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1722.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    386
_cell_measurement_theta_min      2.231
_cell_measurement_theta_max      23.807

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.507
_exptl_crystal_F_000             1268
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.936
_shelx_estimated_absorpt_T_min   0.720
_shelx_estimated_absorpt_T_max   0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_T_max  0.891
_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            8614
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.232
_diffrn_reflns_theta_max         26.119
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1714
_reflns_number_gt                1347
_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)+(0.0631P)²+0.6477P] 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         1714
_refine_ls_number_parameters     150
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.1080
_refine_ls_wR_factor_gt          0.0991
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.062
_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
O1 O 0.6208(2) 0.0067(5) 0.4305(4) 0.0201(9) Uani 1 1 d . . . . .
O5 O 0.5392(2) -0.2337(4) 0.5215(4) 0.0237(10) Uani 1 1 d . . . . .
O6 O 0.5516(3) -0.3358(5) 0.7157(4) 0.0298(11) Uani 1 1 d . . . . .
Ru1 Ru 0.48371(3) 0.06146(5) 0.59146(4) 0.01371(18) Uani 1 1 d . . . . .
Ni1 Ni 0.750000 0.250000 0.68531(10) 0.0241(3) Uani 1 2 d S T P . .
O4 O 0.5050(2) -0.1146(5) 0.7039(4) 0.0202(9) Uani 1 1 d . . . . .
O3 O 0.7038(2) 0.1266(5) 0.5421(4) 0.0256(10) Uani 1 1 d . . . . .
O2 O 0.5891(2) 0.1261(5) 0.6139(4) 0.0217(9) Uani 1 1 d . . . . .
O7 O 0.7098(3) 0.1169(7) 0.8269(5) 0.0555(17) Uani 1 1 d . . . . .
H7B H 0.699910 0.164804 0.896217 0.083 Uiso 1 1 d R U . . .
H7C H 0.671270 0.077783 0.797867 0.083 Uiso 1 1 d R U . . .
C2 C 0.5311(3) -0.2291(7) 0.6493(6) 0.0209(14) Uani 1 1 d . . . . .
C1 C 0.6386(3) 0.0866(6) 0.5293(5) 0.0184(13) Uani 1 1 d . . . . .
O8 O 0.6578(3) 0.3858(5) 0.6819(5) 0.0396(13) Uani 1 1 d . . . . .
H8B H 0.621586 0.334775 0.659807 0.059 Uiso 1 1 d R U . . .
H8C H 0.650226 0.421785 0.758159 0.059 Uiso 1 1 d R U . . .
Na1 Na 0.5793(4) -0.5202(7) 0.4342(6) 0.0519(17) Uani 0.5 1 d . . P . .
O9 O 0.728(3) 0.714(6) 0.586(4) 0.22(2) Uani 0.5 1 d . U P . .
O9' O 0.7071(12) 0.682(3) 0.495(3) 0.138(9) Uani 0.5 1 d . U P . .
O10 O 0.718(4) 0.805(7) 0.762(6) 0.20(3) Uani 0.25 1 d . U P . .
O10' O 0.7095(19) 0.652(4) 0.748(4) 0.096(11) Uani 0.25 1 d . U 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
O1 C1 1.290(7) . ?
O1 Ru1 2.022(4) 5_656 ?
O5 C2 1.308(7) . ?
O5 Ru1 2.012(4) 5_656 ?
O5 Na1 2.897(8) . ?
O6 C2 1.255(7) . ?
O6 Ru1 2.273(4) 3_646 ?
Ru1 O2 2.027(4) . ?
Ru1 O4 2.032(4) . ?
Ru1 Ru1 2.2611(9) 5_656 ?
Ni1 O7 2.034(5) 2_655 ?
Ni1 O7 2.034(5) . ?
Ni1 O3 2.035(4) . ?
Ni1 O3 2.035(4) 2_655 ?
Ni1 O8 2.103(5) 2_655 ?
Ni1 O8 2.103(5) . ?
O4 C2 1.290(7) . ?
O4 Na1 2.981(8) 7_556 ?
O3 C1 1.254(7) . ?
O2 C1 1.300(7) . ?
O7 Na1 2.769(8) 7_556 ?
O7 H7B 0.8523 . ?
O7 H7C 0.8441 . ?
O8 H8B 0.8430 . ?
O8 H8C 0.8548 . ?
Na1 Na1 3.209(14) 5_646 ?
O9 O9 1.04(10) 2_665 ?
O9 O9' 1.78(5) 2_665 ?
O10 O10' 1.38(7) 2_665 ?
O10 O10 1.55(12) 2_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 Ru1 120.2(4) . 5_656 ?
C2 O5 Ru1 121.2(4) . 5_656 ?
C2 O5 Na1 111.3(4) . . ?
Ru1 O5 Na1 127.4(2) 5_656 . ?
C2 O6 Ru1 135.2(4) . 3_646 ?
O5 Ru1 O1 89.38(18) 5_656 5_656 ?
O5 Ru1 O2 91.51(18) 5_656 . ?
O1 Ru1 O2 178.98(17) 5_656 . ?
O5 Ru1 O4 178.77(18) 5_656 . ?
O1 Ru1 O4 89.45(17) 5_656 . ?
O2 Ru1 O4 89.65(17) . . ?
O5 Ru1 Ru1 89.21(12) 5_656 5_656 ?
O1 Ru1 Ru1 89.98(11) 5_656 5_656 ?
O2 Ru1 Ru1 89.56(11) . 5_656 ?
O4 Ru1 Ru1 90.37(12) . 5_656 ?
O5 Ru1 O6 95.72(16) 5_656 3_656 ?
O1 Ru1 O6 87.63(16) 5_656 3_656 ?
O2 Ru1 O6 92.75(16) . 3_656 ?
O4 Ru1 O6 84.64(16) . 3_656 ?
Ru1 Ru1 O6 174.49(11) 5_656 3_656 ?
O7 Ni1 O7 89.9(3) 2_655 . ?
O7 Ni1 O3 176.0(2) 2_655 . ?
O7 Ni1 O3 90.85(19) . . ?
O7 Ni1 O3 90.85(19) 2_655 2_655 ?
O7 Ni1 O3 176.0(2) . 2_655 ?
O3 Ni1 O3 88.7(2) . 2_655 ?
O7 Ni1 O8 95.0(2) 2_655 2_655 ?
O7 Ni1 O8 86.4(2) . 2_655 ?
O3 Ni1 O8 89.00(19) . 2_655 ?
O3 Ni1 O8 89.67(18) 2_655 2_655 ?
O7 Ni1 O8 86.4(2) 2_655 . ?
O7 Ni1 O8 95.0(2) . . ?
O3 Ni1 O8 89.67(18) . . ?
O3 Ni1 O8 89.00(19) 2_655 . ?
O8 Ni1 O8 178.1(3) 2_655 . ?
C2 O4 Ru1 119.4(4) . . ?
C2 O4 Na1 121.0(4) . 7_556 ?
Ru1 O4 Na1 101.0(2) . 7_556 ?
C1 O3 Ni1 129.4(4) . . ?
C1 O2 Ru1 120.1(4) . . ?
Ni1 O7 Na1 141.8(3) . 7_556 ?
Ni1 O7 H7B 110.2 . . ?
Na1 O7 H7B 70.2 7_556 . ?
Ni1 O7 H7C 108.3 . . ?
Na1 O7 H7C 44.1 7_556 . ?
H7B O7 H7C 109.7 . . ?
O6 C2 O4 121.9(5) . . ?
O6 C2 O5 118.3(5) . . ?
O4 C2 O5 119.7(5) . . ?
O3 C1 O1 119.3(5) . . ?
O3 C1 O2 120.5(5) . . ?
O1 C1 O2 120.1(5) . . ?
Ni1 O8 H8B 107.1 . . ?
Ni1 O8 H8C 110.4 . . ?
H8B O8 H8C 109.6 . . ?
O7 Na1 O5 129.4(3) 7 . ?
O7 Na1 O4 102.6(2) 7 7 ?
O5 Na1 O4 75.0(2) . 7 ?
O7 Na1 Na1 167.8(4) 7 5_646 ?
O5 Na1 Na1 62.5(2) . 5_646 ?
O4 Na1 Na1 82.4(3) 7 5_646 ?
O9 O9 O9' 31.1(14) 2_665 2_665 ?
O10' O10 O10 58(4) 2_665 2_665 ?

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
_geom_hbond_publ_flag
O7 H7B O3 0.85 2.44 3.235(7) 155.5 7_566 yes
O7 H7C O2 0.84 2.44 3.090(6) 134.5 . yes
O8 H8B O2 0.84 2.08 2.804(6) 143.8 . yes
O8 H8C O1 0.85 1.95 2.799(6) 172.8 7_566 yes

_refine_diff_density_max         1.467
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.163

