data_2003153
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     1998
_journal_volume     B54
_journal_page_first     613
_journal_page_last     625
_chemical_formula_moiety     'N1 H4,N6 H18 Ru1,2(Cl1 O4),2Cl'
_chemical_formula_sum     'Cl4 H22 N7 O8 Ru1'
_chemical_formula_iupac     'N H4[Ru(N H3)6],2(Cl O4),2Cl'
_chemical_formula_weight     491.12
_symmetry_cell_setting     trigonal
_symmetry_space_group_name_H-M     'R-3m'
_symmetry_space_group_name_Hall     '-R 3 2"'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-y, x-y, z'
    '-x+y, -x, z'
    'y, x, -z'
    'x-y, -y, -z'
    '-x, -x+y, -z'
    'x+2/3, y+1/3, z+1/3'
    '-y+2/3, x-y+1/3, z+1/3'
    '-x+y+2/3, -x+1/3, z+1/3'
    'y+2/3, x+1/3, -z+1/3'
    'x-y+2/3, -y+1/3, -z+1/3'
    '-x+2/3, -x+y+1/3, -z+1/3'
    'x+1/3, y+2/3, z+2/3'
    '-y+1/3, x-y+2/3, z+2/3'
    '-x+y+1/3, -x+2/3, z+2/3'
    'y+1/3, x+2/3, -z+2/3'
    'x-y+1/3, -y+2/3, -z+2/3'
    '-x+1/3, -x+y+2/3, -z+2/3'
    '-x, -y, -z'
    'y, -x+y, -z'
    'x-y, x, -z'
    '-y, -x, z'
    '-x+y, y, z'
    'x, x-y, z'
    '-x+2/3, -y+1/3, -z+1/3'
    'y+2/3, -x+y+1/3, -z+1/3'
    'x-y+2/3, x+1/3, -z+1/3'
    '-y+2/3, -x+1/3, z+1/3'
    '-x+y+2/3, y+1/3, z+1/3'
    'x+2/3, x-y+1/3, z+1/3'
    '-x+1/3, -y+2/3, -z+2/3'
    'y+1/3, -x+y+2/3, -z+2/3'
    'x-y+1/3, x+2/3, -z+2/3'
    '-y+1/3, -x+2/3, z+2/3'
    '-x+y+1/3, y+2/3, z+2/3'
    'x+1/3, x-y+2/3, z+2/3'
_cell_length_a     7.1290(10)
_cell_length_b     7.1290(10)
_cell_length_c     27.560(4)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     120.00
_cell_volume     1213.0(3)
_cell_formula_units_Z     3
_cell_measurement_reflns_used     18
_cell_measurement_theta_min     16.4
_cell_measurement_theta_max     20.3
_cell_measurement_temperature     293(2)
_exptl_crystal_description     Plate
_exptl_crystal_colour     Brown
_exptl_crystal_size_max     0.20
_exptl_crystal_size_mid     0.20
_exptl_crystal_size_min     0.20
_exptl_crystal_density_diffrn     2.017
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     741
_exptl_absorpt_coefficient_mu     1.673
_exptl_absorpt_correction_type     Gaussian
_exptl_absorpt_correction_T_min     0.7210
_exptl_absorpt_correction_T_max     0.7537
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Siemens P3/P4'
_diffrn_measurement_method     '\w/2\q'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     682
_diffrn_reflns_av_R_equivalents     0.0249
_diffrn_reflns_av_sigmaI/netI     0.0191
_diffrn_reflns_theta_min     2.22
_diffrn_reflns_theta_max     25.03
_diffrn_reflns_theta_full     25.03
_diffrn_measured_fraction_theta_max     0.332
_diffrn_measured_fraction_theta_full     0.332
_diffrn_reflns_limit_h_min     -6
_diffrn_reflns_limit_h_max     7
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     8
_diffrn_reflns_limit_l_min     0
_diffrn_reflns_limit_l_max     32
_diffrn_standards_number     3
_diffrn_standards_interval_count     100
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     0.8
_reflns_number_total     306
_reflns_number_gt     303
_reflns_threshold_expression     >2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0194
_refine_ls_R_factor_gt     0.0187
_refine_ls_wR_factor_ref     0.0457
_refine_ls_goodness_of_fit_ref     1.169
_refine_ls_restrained_S_all     1.112
_refine_ls_number_reflns     306
_refine_ls_number_parameters     41
_refine_ls_number_restraints     28
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme
         'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+3.7667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_shift/su_max     0.015
_refine_ls_shift/su_mean     0.001
_refine_diff_density_max     0.300
_refine_diff_density_min     -0.489
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 1983)'
_refine_ls_extinction_coef     0.0064(5)
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'
    'Cl' 'Cl' 0.1484 0.1585
                         '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_
    _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_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ru 0.0000 0.0000 0.0000 0.0142(2) Uani d S 1 . . Ru
    N 0.1391(2) -0.1391(2) -0.04354(8) 0.0322(6) Uani d SD 1 . . N
    H(1) 0.197(2) -0.197(2) -0.0240(12) 0.045(9) Uiso d SPD 0.50 . . H
    H(2) 0.244(3) -0.041(4) -0.0625(4) 0.045(9) Uiso d PD 0.50 . . H
    H(1') 0.130(4) -0.130(4) -0.0758(6) 0.045(9) Uiso d SPD 0.50 . . H
    H(2') 0.279(3) -0.076(3) -0.0354(10) 0.045(9) Uiso d PD 0.50 . . H
    Cl 0.0000 0.0000 0.18601(3) 0.0220(3) Uani d S 1 . . Cl
    O(1) 0.0000 0.0000 0.13400(12) 0.0494(12) Uani d S 1 . . O
    O(2) 0.10914(17) -0.10914(17) 0.20377(7) 0.0392(6) Uani d S 1 . . O
    Cl(1) 0.0000 0.0000 0.37594(4) 0.0296(3) Uani d S 1 . . Cl
    N(1) 0.0000 0.0000 0.5000 0.0291(13) Uani d SD 1 . . N
    H(3) 0.0000 0.0000 0.5334(7) 0.044 Uiso d SPD 0.50 . . H
    H(4) 0.0702(15) -0.0702(15) 0.4889(2) 0.044 Uiso d SPD 0.50 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Ru 0.0158(3) 0.0158(3) 0.0109(3) 0.00792(13) 0.000 0.000
    N 0.0423(11) 0.0423(11) 0.0233(11) 0.0297(13) 0.0026(5) -0.0026(5)
    Cl 0.0248(4) 0.0248(4) 0.0164(5) 0.0124(2) 0.000 0.000
    O(1) 0.0671(19) 0.0671(19) 0.0140(16) 0.0336(9) 0.000 0.000
    O(2) 0.0450(10) 0.0450(10) 0.0409(11) 0.0326(11) -0.0014(5) 0.0014(5)
    Cl(1) 0.0304(4) 0.0304(4) 0.0281(6) 0.0152(2) 0.000 0.000
    N(1) 0.0275(19) 0.0275(19) 0.032(3) 0.0137(10) 0.000 0.000