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#$Date: 2020-05-06 02:47:36 +0300 (Wed, 06 May 2020) $
#$Revision: 251789 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/04/7240451.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_7240451
loop_
_publ_author_name
'Kostin, Gennadiy'
'Filatov, Evgeny'
'Pishchur, Denis P.'
'Kuratieva, Natalia'
'Korenev, Sergey'
_publ_section_title
;
 Phase transformations in a double complex salt of ruthenium nitrosyl
 anion with tetraamine-palladium cation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00441C
_journal_year                    2020
_chemical_formula_moiety         'H13 N9 O10 Pd Ru'
_chemical_formula_sum            'H13 N9 O10 Pd Ru'
_chemical_formula_weight         506.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           10
_space_group_name_Hall           '-P 2y'
_space_group_name_H-M_alt        'P 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-01-24 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.148(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.851(2)
_cell_length_b                   7.792(2)
_cell_length_c                   12.456(3)
_cell_measurement_reflns_used    2355
_cell_measurement_temperature    383(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.62
_cell_volume                     735.5(3)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      383(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker Apex DUO CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6160
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         27.833
_diffrn_reflns_theta_min         1.694
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_description       plate
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_exptl_transmission_factor_max   0.786
_exptl_transmission_factor_min   0.654
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1837
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0156P)²+2.5446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1333
_reflns_number_total             1837
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            d0ce00441c2.cif
_cod_data_source_block           kru217m
_cod_original_sg_symbol_H-M      'P 2/m'
_cod_database_code               7240451
_shelx_shelxl_version_number     2014/7
_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   0.595
_shelx_estimated_absorpt_t_max   0.934
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'-x, -y, -z'
'x, -y, z'
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
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'
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_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_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
