#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/58/2205844.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2205844
loop_
_publ_author_name
'Il'in, Maxim A.'
'Kuratieva, Natalia V.'
'Kirichenko, Olga A.'
'Baidina, Iraida A.'
'Naumov, Dmirty Yu.'
'Korolkow, Ilya V.'
'Emel'yanov, Vyacheslav A.'
_publ_section_title
;
 Tetraamminehydroxonitrosylruthenium(III) tetranitropalladate(II)
 monohydrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i126
_journal_page_last               i128
_journal_paper_doi               10.1107/S1600536805016673
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ru (O H) (N H3)4 (N O)] [Pd (N O2)4], H2 O'
_chemical_formula_moiety         'H13 N5 O2 Ru 2+, N4 O8 Pd 2-, H2 O'
_chemical_formula_sum            'H15 N9 O11 Pd Ru'
_chemical_formula_weight         524.68
_chemical_name_systematic
;
Tetraamminehydroxonitrosylruthenium(III) tetranitropalladate(II) monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.1470(10)
_cell_angle_beta                 115.3900(10)
_cell_angle_gamma                108.7280(10)
_cell_formula_units_Z            2
_cell_length_a                   9.0710(3)
_cell_length_b                   10.0861(5)
_cell_length_c                   10.1864(3)
_cell_measurement_reflns_used    4128
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.51
_cell_measurement_theta_min      2.38
_cell_volume                     741.78(5)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ball & Stick (BS) (Ozawa & Kang, 2004)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker--Nonius X8APEX CCD area-detector'
_diffrn_measurement_method       φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4633
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.303
_exptl_absorpt_correction_T_max  0.7696
_exptl_absorpt_correction_T_min  0.6434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Blessing, 1995)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    2.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.469
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0239P)²+0.2798P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0449
_reflns_number_gt                2535
_reflns_number_total             2756
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ac6171.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (19
times).

'_geom_angle_publ_flag' value 'Yes' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (20 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (19
times).

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (20
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2205844
_cod_database_fobs_code          2205844
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Ru1 -0.00142(2) 0.822966(19) 0.28190(2) 0.01188(6) Uani d . 1 Ru
Pd1 0.5000 0.5000 0.5000 0.01480(7) Uani d S 1 Pd
Pd2 0.5000 0.0000 0.0000 0.01464(7) Uani d S 1 Pd
O1 -0.1482(2) 0.91272(18) 0.32070(18) 0.0155(3) Uani d . 1 O
H1 -0.2550 0.8698 0.2429 0.019 Uiso calc R 1 H
N1 -0.2342(3) 0.6131(2) 0.1541(2) 0.0181(4) Uani d . 1 N
H1A -0.2717 0.5871 0.0509 0.027 Uiso calc R 1 H
H1B -0.3249 0.6194 0.1676 0.027 Uiso calc R 1 H
H1C -0.2065 0.5420 0.1885 0.027 Uiso calc R 1 H
N2 -0.0799(3) 0.8803(2) 0.0824(2) 0.0161(4) Uani d . 1 N
H2A -0.0172 0.8635 0.0369 0.024 Uiso calc R 1 H
H2B -0.0548 0.9793 0.1103 0.024 Uiso calc R 1 H
H2C -0.2016 0.8230 0.0136 0.024 Uiso calc R 1 H
N3 0.2128(3) 1.0431(2) 0.4139(2) 0.0184(4) Uani d . 1 N
H3A 0.3173 1.0437 0.4230 0.028 Uiso calc R 1 H
H3B 0.2289 1.0741 0.5106 0.028 Uiso calc R 1 H
H3C 0.1845 1.1063 0.3650 0.028 Uiso calc R 1 H
N4 0.0561(3) 0.7846(2) 0.4916(2) 0.0164(4) Uani d . 1 N
H4A -0.0424 0.7050 0.4743 0.025 Uiso calc R 1 H
H4B 0.0816 0.8680 0.5652 0.025 Uiso calc R 1 H
H4C 0.1539 0.7642 0.5256 0.025 Uiso calc R 1 H
N 0.1227(3) 0.7424(2) 0.2373(2) 0.0192(4) Uani d . 1 N
O 0.1878(3) 0.6816(2) 0.1895(2) 0.0365(5) Uani d . 1 O
N5 0.4345(3) 0.5241(2) 0.2926(2) 0.0182(4) Uani d . 1 N
N6 0.6647(3) 0.4096(2) 0.4783(2) 0.0207(4) Uani d . 1 N
O51 0.2904(2) 0.42761(19) 0.1719(2) 0.0252(4) Uani d . 1 O
O52 0.5378(3) 0.6320(2) 0.2849(2) 0.0312(4) Uani d . 1 O
O61 0.6177(3) 0.2754(2) 0.4635(3) 0.0369(5) Uani d . 1 O
O62 0.7966(3) 0.4812(3) 0.4807(3) 0.0560(7) Uani d . 1 O
N7 0.4323(3) -0.0112(2) 0.1660(2) 0.0180(4) Uani d . 1 N
N8 0.5986(3) 0.2263(2) 0.0803(2) 0.0194(4) Uani d . 1 N
O71 0.5217(3) -0.0422(2) 0.2758(2) 0.0344(5) Uani d . 1 O
O72 0.3036(2) 0.0107(2) 0.1525(2) 0.0300(4) Uani d . 1 O
O81 0.4924(2) 0.2824(2) 0.0455(3) 0.0339(5) Uani d . 1 O
O82 0.7650(2) 0.3096(2) 0.1623(2) 0.0301(4) Uani d . 1 O
O1W 0.0408(3) 0.2095(2) 0.2116(2) 0.0252(4) Uani d . 1 O
H2 -0.031(5) 0.232(4) 0.196(4) 0.035(10) Uiso d . 1 H
H3 0.124(5) 0.286(4) 0.219(4) 0.048(11) Uiso d . 1 H
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ru1 N O . . 171.8(2) yes
N Ru1 O1 . . 176.99(8) yes
O1 Ru1 N1 . . 89.19(7) yes
O1 Ru1 N2 . . 84.90(7) yes
O1 Ru1 N3 . . 84.35(7) yes
O1 Ru1 N4 . . 85.85(7) yes
N Ru1 N1 . . 89.84(9) yes
N Ru1 N2 . . 92.27(9) yes
N Ru1 N3 . . 96.62(9) yes
N Ru1 N4 . . 97.00(8) yes
N1 Ru1 N2 . . 90.39(8) yes
N1 Ru1 N4 . . 90.49(8) yes
N2 Ru1 N3 . . 89.00(8) yes
N3 Ru1 N4 . . 89.08(8) yes
N5 Pd1 N6 . . 89.53(8) yes
N7 Pd2 N8 . . 90.52(8) yes
O51 N5 O52 . . 120.1(2) yes
O61 N6 O62 . . 121.9(2) yes
O71 N7 O72 . . 121.9(2) yes
O81 N8 O82 . . 119.35(19) yes
N2 Ru1 N4 . . 170.69(7) ?
N1 Ru1 N3 . . 173.54(8) ?
N5 Pd1 N5 2_666 . 180.0 ?
N5 Pd1 N6 2_666 . 90.47(8) ?
N5 Pd1 N6 2_666 2_666 89.53(8) ?
N5 Pd1 N6 . 2_666 90.47(8) ?
N6 Pd1 N6 . 2_666 180.0000(10) ?
N8 Pd2 N8 2_655 . 180.00(14) ?
N8 Pd2 N7 2_655 2_655 90.52(8) ?
N8 Pd2 N7 . 2_655 89.48(8) ?
N8 Pd2 N7 2_655 . 89.48(8) ?
N7 Pd2 N7 2_655 . 180.00(19) ?
Ru1 O1 H1 . . 109.5 ?
Ru1 N1 H1A . . 109.5 ?
Ru1 N1 H1B . . 109.5 ?
H1A N1 H1B . . 109.5 ?
Ru1 N1 H1C . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
Ru1 N2 H2A . . 109.5 ?
Ru1 N2 H2B . . 109.5 ?
H2A N2 H2B . . 109.5 ?
Ru1 N2 H2C . . 109.5 ?
H2A N2 H2C . . 109.5 ?
H2B N2 H2C . . 109.5 ?
Ru1 N3 H3A . . 109.5 ?
Ru1 N3 H3B . . 109.5 ?
H3A N3 H3B . . 109.5 ?
Ru1 N3 H3C . . 109.5 ?
H3A N3 H3C . . 109.5 ?
H3B N3 H3C . . 109.5 ?
Ru1 N4 H4A . . 109.5 ?
Ru1 N4 H4B . . 109.5 ?
H4A N4 H4B . . 109.5 ?
Ru1 N4 H4C . . 109.5 ?
H4A N4 H4C . . 109.5 ?
H4B N4 H4C . . 109.5 ?
O52 N5 Pd1 . . 120.15(16) ?
O51 N5 Pd1 . . 119.78(15) ?
O62 N6 Pd1 . . 121.64(17) ?
O61 N6 Pd1 . . 116.50(17) ?
O72 N7 Pd2 . . 119.12(16) ?
O71 N7 Pd2 . . 119.01(16) ?
O81 N8 Pd2 . . 119.49(15) ?
O82 N8 Pd2 . . 121.15(15) ?
H2 O1W H3 . . 103(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ru1 N . 1.742(2) yes
N O . 1.155(3) yes
Ru1 O1 . 1.9618(15) yes
Ru1 N1 . 2.1062(19) yes
Ru1 N2 . 2.0995(18) yes
Ru1 N3 . 2.1095(19) yes
Ru1 N4 . 2.1091(19) yes
Pd1 N5 . 2.018(2) yes
Pd1 N6 . 2.049(2) yes
N5 O51 . 1.245(3) yes
N5 O52 . 1.228(3) yes
N6 O61 . 1.241(3) yes
N6 O62 . 1.170(3) yes
Pd2 N7 . 2.040(2) yes
Pd2 N8 . 2.020(2) yes
N7 O71 . 1.231(3) yes
N7 O72 . 1.212(3) yes
N8 O81 . 1.226(3) yes
N8 O82 . 1.241(3) yes
Pd1 N5 2_666 2.018(2) ?
Pd1 N6 2_666 2.049(2) ?
Pd2 N7 2_655 2.040(2) ?
Pd2 N8 2_655 2.020(2) ?
O1 H1 . 0.8400 ?
N1 H1A . 0.9100 ?
N1 H1B . 0.9100 ?
N1 H1C . 0.9100 ?
N2 H2A . 0.9100 ?
N2 H2B . 0.9100 ?
N2 H2C . 0.9100 ?
N3 H3A . 0.9100 ?
N3 H3B . 0.9100 ?
N3 H3C . 0.9100 ?
N4 H4A . 0.9100 ?
N4 H4B . 0.9100 ?
N4 H4C . 0.9100 ?
O1W H2 . 0.72(3) ?
O1W H3 . 0.85(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1 O81 2_565 0.84 2.55 3.319(3) 153
O1 H1 O71 1_465 0.84 2.58 3.025(2) 115
N1 H1A O51 2_565 0.91 2.18 3.064(3) 165
N1 H1B O52 1_455 0.91 2.08 2.936(3) 157
N1 H1C O82 1_455 0.91 2.23 3.075(3) 154
N2 H2A O72 1_565 0.91 2.39 2.990(3) 123
N2 H2B O1W 1_565 0.91 2.07 2.974(3) 170
N2 H2B O1W 1_565 0.91 2.07 2.974(3) 170
N2 H2C O81 2_565 0.91 2.25 3.085(3) 152
N2 H2C O51 2_565 0.91 2.51 3.020(3) 116
N3 H3B O1 2_576 0.91 2.14 2.992(3) 156
N3 H3B O71 2_666 0.91 2.54 3.048(3) 116
N3 H3C O1W 1_565 0.91 2.22 3.105(3) 165
N4 H4A O62 1_455 0.91 2.29 3.154(3) 158
N4 H4B O1 2_576 0.91 2.06 2.934(3) 161
N4 H4C O61 2_666 0.91 2.19 3.069(3) 161
O1W H2 O82 1_455 0.72(3) 2.15(4) 2.873(3) 177(4)
O1W H3 O51 . 0.85(4) 2.00(4) 2.833(3) 164(3)
