#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/83/2018327.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_2018327
loop_
_publ_author_name
'Buron-Le Cointe, Marylise'
'Cormary, Beno\?ît'
'Toupet, Loïc'
'Malfant, Isabelle'
_publ_section_title
;
 The three-dimensional intermolecular network formed via water
 molecules in
 trans-bis(nitrito-κN)tetrakis(pyridine-κN)ruthenium(II)
 dihydrate
;
_journal_coeditor_code           MX3053
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m375
_journal_page_last               m377
_journal_paper_doi               10.1107/S0108270111044672
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ru (N O2)2 (C5 H5 N1)4] , 2H2 O'
_chemical_formula_moiety         'C20 H20 N6 O4 Ru, 2(H2 O)'
_chemical_formula_sum            'C20 H24 N6 O6 Ru'
_chemical_formula_weight         545.52
_chemical_name_systematic
;
trans-bis(nitrito-κN)tetrakis(pyridine-κN)ruthenium(II)
dihydrate
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.3418(2)
_cell_length_b                   16.3418(2)
_cell_length_c                   16.6448(2)
_cell_measurement_reflns_used    3452
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.0
_cell_volume                     4445.07(9)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 19.64
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Oxford Xcalibur diffractometer with Sapphire 3 CCD area detector'
_diffrn_measurement_method       ω
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17299
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.94118
_exptl_absorpt_correction_T_min  0.88573
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(PLATON; Spek, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1221
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0301P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0491
_reflns_number_gt                907
_reflns_number_total             1221
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            mx3053.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               2018327
_cod_database_fobs_code          2018327
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'y+3/4, x+1/4, -z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'y+5/4, x+3/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z-1/2'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-y-3/4, -x-1/4, z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'
'-y-1/4, -x+1/4, z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
O O2 0.16048(10) 0.0000 0.2500 0.0329(4) Uani d SD 1 2
H H2A 0.1273(10) 0.0223(11) 0.2141(11) 0.049 Uiso d D 1 1
Ru Ru1 0.0000 0.2500 0.1250 0.01115(9) Uani d S 1 4
N N1 -0.05987(7) 0.18279(7) 0.21495(7) 0.0143(3) Uani d . 1 1
N N2 0.08869(7) 0.16131(7) 0.1250 0.0170(4) Uani d S 1 2
O O1 0.07118(7) 0.08656(6) 0.13059(6) 0.0244(3) Uani d . 1 1
C C1 -0.14074(9) 0.16593(9) 0.21282(9) 0.0180(3) Uani d . 1 1
H H1 -0.1728 0.1890 0.1709 0.022 Uiso calc R 1 1
C C2 -0.17878(10) 0.11683(10) 0.26858(9) 0.0229(4) Uani d . 1 1
H H2 -0.2359 0.1067 0.2650 0.028 Uiso calc R 1 1
C C3 -0.13324(11) 0.08240(10) 0.32987(9) 0.0257(4) Uani d . 1 1
H H3 -0.1582 0.0479 0.3688 0.031 Uiso calc R 1 1
C C4 -0.05066(10) 0.09936(9) 0.33311(9) 0.0226(4) Uani d . 1 1
H H4 -0.0176 0.0767 0.3745 0.027 Uiso calc R 1 1
C C5 -0.01667(9) 0.14948(9) 0.27567(9) 0.0184(3) Uani d . 1 1
H H5 0.0402 0.1612 0.2790 0.022 Uiso calc R 1 1
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'
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N2 Ru1 N2 . 2 180.0
N2 Ru1 N1 . 6_455 92.31(3)
N2 Ru1 N1 2 6_455 87.69(3)
N2 Ru1 N1 . 2 92.31(3)
N2 Ru1 N1 2 2 87.68(3)
N1 Ru1 N1 6_455 2 175.37(6)
N2 Ru1 N1 . 5 87.69(3)
N2 Ru1 N1 2 5 92.31(3)
N1 Ru1 N1 6_455 5 88.99(6)
N1 Ru1 N1 2 5 91.20(6)
N2 Ru1 N1 . . 87.68(3)
N2 Ru1 N1 2 . 92.32(3)
N1 Ru1 N1 6_455 . 91.20(6)
N1 Ru1 N1 2 . 88.99(6)
N1 Ru1 N1 5 . 175.37(6)
C5 N1 C1 . . 116.75(13)
C5 N1 Ru1 . . 120.14(10)
C1 N1 Ru1 . . 122.97(10)
O1 N2 O1 5 . 116.56(17)
O1 N2 Ru1 5 . 121.72(9)
O1 N2 Ru1 . . 121.72(9)
N1 C1 C2 . . 122.92(14)
N1 C1 H1 . . 118.5
C2 C1 H1 . . 118.5
C1 C2 C3 . . 119.48(15)
C1 C2 H2 . . 120.3
C3 C2 H2 . . 120.3
C4 C3 C2 . . 118.29(15)
C4 C3 H3 . . 120.9
C2 C3 H3 . . 120.9
C5 C4 C3 . . 119.18(15)
C5 C4 H4 . . 120.4
C3 C4 H4 . . 120.4
N1 C5 C4 . . 123.36(14)
N1 C5 H5 . . 118.3
C4 C5 H5 . . 118.3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
O2 H2A . 0.885(14)
Ru1 N2 . 2.0496(17)
Ru1 N2 2 2.0496(17)
Ru1 N1 6_455 2.0989(12)
Ru1 N1 2 2.0989(12)
Ru1 N1 5 2.0989(12)
Ru1 N1 . 2.0989(12)
N1 C5 . 1.3476(18)
N1 C1 . 1.3503(18)
N2 O1 5 1.2582(13)
N2 O1 . 1.2582(13)
C1 C2 . 1.375(2)
C1 H1 . 0.9500
C2 C3 . 1.382(2)
C2 H2 . 0.9500
C3 C4 . 1.379(2)
C3 H3 . 0.9500
C4 C5 . 1.376(2)
C4 H4 . 0.9500
C5 H5 . 0.9500
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N2 Ru1 N1 C5 . . 42.63(10)
N2 Ru1 N1 C5 2 . -137.37(10)
N1 Ru1 N1 C5 6_455 . 134.90(12)
N1 Ru1 N1 C5 2 . -49.72(10)
N2 Ru1 N1 C1 . . -132.82(11)
N2 Ru1 N1 C1 2 . 47.18(11)
N1 Ru1 N1 C1 6_455 . -40.55(10)
N1 Ru1 N1 C1 2 . 134.82(13)
N1 Ru1 N2 O1 6_455 5 129.46(6)
N1 Ru1 N2 O1 2 5 -50.54(6)
N1 Ru1 N2 O1 5 5 40.56(6)
N1 Ru1 N2 O1 . 5 -139.43(6)
N1 Ru1 N2 O1 6_455 . -50.54(6)
N1 Ru1 N2 O1 2 . 129.46(6)
N1 Ru1 N2 O1 5 . -139.43(6)
N1 Ru1 N2 O1 . . 40.57(6)
C5 N1 C1 C2 . . -0.6(2)
Ru1 N1 C1 C2 . . 175.03(11)
N1 C1 C2 C3 . . -0.2(2)
C1 C2 C3 C4 . . 0.5(2)
C2 C3 C4 C5 . . -0.1(2)
C1 N1 C5 C4 . . 1.1(2)
Ru1 N1 C5 C4 . . -174.67(12)
C3 C4 C5 N1 . . -0.8(2)
