#------------------------------------------------------------------------------
#$Date: 2021-07-31 11:12:04 +0300 (Sat, 31 Jul 2021) $
#$Revision: 267854 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/42/1564284.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1564284
loop_
_publ_author_name
'Wang, Lin-Lin'
'Ding, Tuo'
'Xue, Xiang-Xian'
'Yang, Jian-Hui'
'Liu, Bin'
_publ_section_title
;
 A series of C-Shaped heterometallic Diruthenium(II,III) phosphates:
 NH4[{M(H2O)5}2Ru2(HPO4)2(PO4)2(H2O)2]·4H2O (M = Mg,
 Co, Ni and Zn)
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119730
_journal_paper_doi               10.1016/j.ica.2020.119730
_journal_volume                  510
_journal_year                    2020
_chemical_formula_moiety         'H26 Ni2 O28 P4 Ru2, H4 N, 4(H2 O)'
_chemical_formula_sum            'H38 N Ni2 O32 P4 Ru2'
_chemical_formula_weight         1007.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2254(12)
_cell_length_b                   22.192(2)
_cell_length_c                   10.4785(11)
_cell_measurement_reflns_used    8024
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.278
_cell_measurement_theta_min      2.560
_cell_volume                     2842.9(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1261
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15075
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.280
_diffrn_reflns_theta_min         1.835
_exptl_absorpt_coefficient_mu    2.693
_exptl_absorpt_correction_T_max  0.584
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.354
_exptl_crystal_description       block
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.662
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.193
_refine_ls_extinction_coef       0.0024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2948
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0692P)²+2.5422P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2680
_reflns_number_total             2948
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Ni2Ru2PO4.cif
_cod_data_source_block           xb2694_0ma_a
_cod_database_code               1564284
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.346
_shelx_estimated_absorpt_t_max   0.615
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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 0.83942(3) 0.250000 0.44102(4) 0.01065(16) Uani 1 2 d S T P . .
Ru2 Ru 0.66910(3) 0.250000 0.53924(4) 0.01132(16) Uani 1 2 d S T P . .
Ni1 Ni 0.85971(4) 0.40410(2) 0.94525(4) 0.01731(18) Uani 1 1 d . . . . .
P1 P 0.82538(7) 0.34504(4) 0.66005(9) 0.0143(2) Uani 1 1 d . . . . .
P2 P 0.68638(8) 0.14927(4) 0.33117(9) 0.0152(2) Uani 1 1 d . . . . .
O16 O 0.9491(3) 0.42735(14) 0.3240(3) 0.0367(7) Uani 1 1 d . . . . .
H16D H 0.964079 0.387780 0.330890 0.044 Uiso 1 1 d R U . . .
H16C H 0.935589 0.442680 0.401920 0.055 Uiso 1 1 d R U . . .
O1 O 0.8993(2) 0.31296(13) 0.5630(2) 0.0203(6) Uani 1 1 d . . . . .
O2 O 0.7128(2) 0.31435(12) 0.6653(3) 0.0226(6) Uani 1 1 d . . . . .
O3 O 0.8780(2) 0.34947(11) 0.7895(2) 0.0199(6) Uani 1 1 d . . . . .
O4 O 0.8087(2) 0.41175(12) 0.6107(3) 0.0230(6) Uani 1 1 d D . . . .
O5 O 0.7935(2) 0.18576(11) 0.3131(2) 0.0198(6) Uani 1 1 d . . . . .
O6 O 0.6107(2) 0.18595(14) 0.4210(3) 0.0259(6) Uani 1 1 d . . . . .
O7 O 0.6285(2) 0.14070(12) 0.2048(3) 0.0239(6) Uani 1 1 d . . . . .
O8 O 0.7133(3) 0.08926(13) 0.3956(3) 0.0350(8) Uani 1 1 d . . . . .
O9 O 1.0163(3) 0.250000 0.3560(4) 0.0284(9) Uani 1 2 d DS T P . .
O10 O 0.5060(3) 0.250000 0.6509(4) 0.0245(9) Uani 1 2 d DS T P . .
O11 O 0.8921(2) 0.33228(13) 1.0665(3) 0.0257(6) Uani 1 1 d . . . . .
H11A H 0.831993 0.317310 1.092177 0.039 Uiso 1 1 d R U . . .
H11C H 0.928713 0.344710 1.130157 0.039 Uiso 1 1 d R U . . .
O12 O 1.0284(2) 0.42210(14) 0.9138(3) 0.0292(6) Uani 1 1 d . . . . .
H12B H 1.058938 0.430421 0.984517 0.044 Uiso 1 1 d R U . . .
H12C H 1.058678 0.391201 0.881337 0.044 Uiso 1 1 d R U . . .
O13 O 0.8224(3) 0.47583(13) 0.8311(3) 0.0369(8) Uani 1 1 d . . . . .
H13B H 0.850096 0.507593 0.862897 0.055 Uiso 1 1 d R U . . .
H13C H 0.848966 0.469904 0.757177 0.055 Uiso 1 1 d R U . . .
O14 O 0.6991(2) 0.38094(14) 0.9693(3) 0.0265(6) Uani 1 1 d . . . . .
H14A H 0.665169 0.410070 1.003935 0.040 Uiso 1 1 d R U . . .
H14B H 0.670679 0.373230 0.897085 0.040 Uiso 1 1 d R U . . .
O15 O 0.8605(3) 0.46325(14) 1.0965(3) 0.0331(7) Uani 1 1 d . . . . .
H15B H 0.906061 0.451338 1.152339 0.050 Uiso 1 1 d R U . . .
H15C H 0.878821 0.498048 1.070179 0.050 Uiso 1 1 d R U . . .
N1 N 0.6377(6) 0.250000 0.8991(6) 0.0452(15) Uani 1 2 d S T P . .
H1D H 0.658835 0.268380 0.832354 0.054 Uiso 0.5 1 d R U P . .
H1A H 0.650505 0.271690 0.964275 0.068 Uiso 0.5 1 d R U P . .
H1B H 0.569435 0.243100 0.894014 0.068 Uiso 0.5 1 d R U P . .
H1C H 0.671975 0.216830 0.905795 0.068 Uiso 0.5 1 d R U P . .
O17 O 0.5411(3) 0.44893(14) 0.8566(3) 0.0402(8) Uani 1 1 d . . . . .
H17B H 0.598405 0.470493 0.851544 0.060 Uiso 1 1 d R U . . .
H17C H 0.503195 0.453284 0.789244 0.060 Uiso 1 1 d R U . . .
H3 H 0.775(5) 0.422(3) 0.543(4) 0.056(19) Uiso 1 1 d D . . . .
H1 H 1.048(5) 0.2833(16) 0.338(6) 0.061(19) Uiso 1 1 d D . . . .
H2 H 0.473(4) 0.2830(14) 0.660(5) 0.037(14) Uiso 1 1 d D . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
P P 0.1023 0.0942 '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'
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
O1 Ru1 O1 86.96(17) . 7_565
O1 Ru1 O5 174.84(11) . .
O1 Ru1 O5 91.84(11) 7_565 .
O1 Ru1 O5 91.84(11) . 7_565
O1 Ru1 O5 174.84(11) 7_565 7_565
O5 Ru1 O5 88.91(15) . 7_565
O1 Ru1 Ru2 92.53(8) . .
O1 Ru1 Ru2 92.53(8) 7_565 .
O5 Ru1 Ru2 92.54(7) . .
O5 Ru1 Ru2 92.54(7) 7_565 .
O1 Ru1 O9 84.64(12) . .
O1 Ru1 O9 84.64(12) 7_565 .
O5 Ru1 O9 90.25(11) . .
O5 Ru1 O9 90.25(11) 7_565 .
Ru2 Ru1 O9 176.09(12) . .
O6 Ru2 O6 89.65(19) 7_565 .
O6 Ru2 O2 174.37(11) 7_565 7_565
O6 Ru2 O2 89.83(13) . 7_565
O6 Ru2 O2 89.83(13) 7_565 .
O6 Ru2 O2 174.37(11) . .
O2 Ru2 O2 90.14(16) 7_565 .
O6 Ru2 O10 90.31(11) 7_565 .
O6 Ru2 O10 90.31(11) . .
O2 Ru2 O10 84.08(11) 7_565 .
O2 Ru2 O10 84.08(11) . .
O6 Ru2 Ru1 92.59(8) 7_565 .
O6 Ru2 Ru1 92.59(8) . .
O2 Ru2 Ru1 93.04(8) 7_565 .
O2 Ru2 Ru1 93.04(8) . .
O10 Ru2 Ru1 175.91(12) . .
O13 Ni1 O14 93.08(13) . .
O13 Ni1 O3 91.09(11) . .
O14 Ni1 O3 93.09(12) . .
O13 Ni1 O15 87.42(13) . .
O14 Ni1 O15 94.02(12) . .
O3 Ni1 O15 172.80(13) . .
O13 Ni1 O11 177.51(12) . .
O14 Ni1 O11 85.11(12) . .
O3 Ni1 O11 90.71(11) . .
O15 Ni1 O11 91.01(12) . .
O13 Ni1 O12 88.81(13) . .
O14 Ni1 O12 175.89(12) . .
O3 Ni1 O12 83.21(12) . .
O15 Ni1 O12 89.71(13) . .
O11 Ni1 O12 93.11(12) . .
O3 P1 O1 112.08(16) . .
O3 P1 O2 112.30(16) . .
O1 P1 O2 110.21(15) . .
O3 P1 O4 106.77(15) . .
O1 P1 O4 107.06(16) . .
O2 P1 O4 108.14(16) . .
O7 P2 O8 112.17(16) . .
O7 P2 O5 110.70(16) . .
O8 P2 O5 109.08(18) . .
O7 P2 O6 108.55(17) . .
O8 P2 O6 108.54(19) . .
O5 P2 O6 107.67(15) . .
H16D O16 H16C 109.5 . .
P1 O1 Ru1 121.59(16) . .
P1 O2 Ru2 121.82(15) . .
P1 O3 Ni1 135.37(17) . .
P1 O4 H3 126(4) . .
P2 O5 Ru1 121.23(14) . .
P2 O6 Ru2 122.12(16) . .
Ru1 O9 H1 120(4) . .
Ru1 O9 H1 120(4) . 7_565
H1 O9 H1 120(8) . 7_565
Ru2 O10 H2 118(4) . .
Ru2 O10 H2 118(4) . 7_565
H2 O10 H2 121(7) . 7_565
Ni1 O11 H11A 109.2 . .
Ni1 O11 H11C 109.4 . .
H11A O11 H11C 109.5 . .
Ni1 O12 H12B 109.3 . .
Ni1 O12 H12C 109.4 . .
H12B O12 H12C 109.5 . .
Ni1 O13 H13B 109.1 . .
Ni1 O13 H13C 109.1 . .
H13B O13 H13C 109.5 . .
Ni1 O14 H14A 109.3 . .
Ni1 O14 H14B 109.5 . .
H14A O14 H14B 109.5 . .
Ni1 O15 H15B 109.6 . .
Ni1 O15 H15C 109.3 . .
H15B O15 H15C 109.5 . .
H1D N1 H1A 109.5 . .
H1D N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
H1D N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
H1D N1 H1D 57.4 . 7_565
H1A N1 H1D 151.2 . 7_565
H1B N1 H1D 99.2 . 7_565
H1C N1 H1D 60.1 . 7_565
H1D N1 H1A 151.3 . 7_565
H1A N1 H1A 69.0 . 7_565
H1B N1 H1A 97.4 . 7_565
H1C N1 H1A 49.6 . 7_565
H1D N1 H1A 109.5 7_565 7_565
H1D N1 H1B 99.2 . 7_565
H1A N1 H1B 97.4 . 7_565
H1B N1 H1B 20.8 . 7_565
H1C N1 H1B 130.2 . 7_565
H1D N1 H1B 109.5 7_565 7_565
H1A N1 H1B 109.5 7_565 7_565
H1D N1 H1C 60.2 . 7_565
H1A N1 H1C 49.6 . 7_565
H1B N1 H1C 130.2 . 7_565
H1C N1 H1C 120.0 . 7_565
H1D N1 H1C 109.5 7_565 7_565
H1A N1 H1C 109.5 7_565 7_565
H1B N1 H1C 109.5 7_565 7_565
H17B O17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 O1 2.031(3) .
Ru1 O1 2.031(3) 7_565
Ru1 O5 2.036(2) .
Ru1 O5 2.036(2) 7_565
Ru1 Ru2 2.3228(6) .
Ru1 O9 2.339(4) .
Ru2 O6 2.016(3) 7_565
Ru2 O6 2.016(3) .
Ru2 O2 2.017(3) 7_565
Ru2 O2 2.017(3) .
Ru2 O10 2.312(4) .
Ni1 O13 2.043(3) .
Ni1 O14 2.045(3) .
Ni1 O3 2.045(3) .
Ni1 O15 2.058(3) .
Ni1 O11 2.076(3) .
Ni1 O12 2.127(3) .
P1 O3 1.504(3) .
P1 O1 1.535(3) .
P1 O2 1.537(3) .
P1 O4 1.581(3) .
P2 O7 1.513(3) .
P2 O8 1.529(3) .
P2 O5 1.551(3) .
P2 O6 1.551(3) .
O16 H16D 0.8999 .
O16 H16C 0.9000 .
O4 H3 0.85(2) .
O9 H1 0.854(19) .
O9 H1 0.854(19) 7_565
O10 H2 0.841(19) .
O10 H2 0.841(19) 7_565
O11 H11A 0.8500 .
O11 H11C 0.8499 .
O12 H12B 0.8500 .
O12 H12C 0.8499 .
O13 H13B 0.8500 .
O13 H13C 0.8500 .
O14 H14A 0.8500 .
O14 H14B 0.8500 .
O15 H15B 0.8500 .
O15 H15C 0.8500 .
N1 H1D 0.8500 .
N1 H1A 0.8501 .
N1 H1B 0.8500 .
N1 H1C 0.8500 .
N1 H1D 0.8499 7_565
N1 H1A 0.8501 7_565
N1 H1B 0.8500 7_565
N1 H1C 0.8501 7_565
O17 H17B 0.8501 .
O17 H17C 0.8500 .
