#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003157.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_2003157
loop_
_publ_author_name
'Figgis, B. N.'
'Sobolev, A. N.'
'Reynolds, P. A.'
_publ_section_title
;
 Phase Transitions and Structures at 10, 92 and 293 K in Eight Trigonal
 Double Salts
 <i>M</i>^I^[<i>M</i>^III^(NH~3~)~6~](ClO~4~)~2~<i>X</i>~2~
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              613
_journal_page_last               625
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          'Rb[Ru(N H3)6],2(Cl O4),2Cl'
_chemical_formula_moiety         'Rb1,N6 H18 Ru1,2(Cl1 O4),2Cl'
_chemical_formula_sum            'Cl4 H18 N6 O8 Rb Ru'
_chemical_formula_weight         558.54
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   7.1040(10)
_cell_length_b                   7.1040(10)
_cell_length_c                   27.408(7)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    92(2)
_cell_measurement_theta_max      20.2
_cell_measurement_theta_min      16.4
_cell_volume                     1197.9(4)
_computing_cell_refinement       'P3/PC (Siemens, 1989)'
_computing_data_collection       'P3/PC (Siemens, 1989)'
_computing_data_reduction        'PROFIT (Streltsov & Zavodnik, 1989)'
_computing_publication_material  'SHELXTL (Sheldrick, 1983)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      92(2)
_diffrn_measured_fraction_theta_full 0.333
_diffrn_measured_fraction_theta_max 0.334
_diffrn_measurement_device_type  'Siemens P3/P4'
_diffrn_measurement_method       \w/2\q
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            24024
_diffrn_reflns_theta_full        55.18
_diffrn_reflns_theta_max         55.18
_diffrn_reflns_theta_min         2.23
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  1.6?
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.719
_exptl_absorpt_correction_T_max  0.5646
_exptl_absorpt_correction_T_min  0.3699
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Trigonal antiprism'
_exptl_crystal_F_000             819
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.143
_refine_diff_density_min         -1.260
_refine_ls_extinction_coef       0.00039(16)
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 1983)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         3462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+2.1148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                3307
_reflns_number_total             3462
_reflns_threshold_expression     >2sigma(I)
_[local]_cod_data_source_file    ta0002.cif
_[local]_cod_data_source_block   Va
_[local]_cod_cif_authors_sg_H-M  R-3
_[local]_cod_chemical_formula_sum_orig 'Cl4 H18 N6 O8 Rb1 Ru1'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2003157
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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'
'-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'
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
Ru 0.0000 0.0000 0.0000 0.00631(2) Uani d S 1 Ru
N 0.16639(14) -0.11335(14) -0.04363(3) 0.01213(13) Uani d . 1 N
H(1) 0.177(6) -0.215(7) -0.0288(9) 0.028(7) Uiso d . 1 H
H(2) 0.290(5) -0.009(5) -0.0534(10) 0.022(6) Uiso d . 1 H
H(3) 0.099(5) -0.187(5) -0.0683(8) 0.022(7) Uiso d . 1 H
Cl 0.0000 0.0000 0.185695(10) 0.00896(4) Uani d S 1 Cl
O(1) 0.0000 0.0000 0.13313(4) 0.0187(2) Uani d S 1 O
O(2) 0.08733(15) -0.13195(15) 0.20358(3) 0.01523(15) Uani d . 1 O
Cl(1) 0.0000 0.0000 0.376242(12) 0.01193(4) Uani d S 1 Cl
Rb 0.0000 0.0000 0.5000 0.01010(3) Uani d S 1 Rb
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 0.00692(3) 0.00692(3) 0.00508(3) 0.003460(10) 0.000 0.000
N 0.0136(3) 0.0153(3) 0.0101(2) 0.0093(3) 0.00089(17) -0.00135(18)
Cl 0.00974(5) 0.00974(5) 0.00740(7) 0.00487(3) 0.000 0.000
O(1) 0.0245(3) 0.0245(3) 0.0072(3) 0.01223(16) 0.000 0.000
O(2) 0.0175(4) 0.0161(4) 0.0166(2) 0.0118(4) 0.0009(2) 0.0021(2)
Cl(1) 0.01227(6) 0.01227(6) 0.01125(9) 0.00614(3) 0.000 0.000
Rb 0.01005(4) 0.01005(4) 0.01021(5) 0.00503(2) 0.000 0.000
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'
Rb Rb -0.9393 2.9676 '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
N Ru N 3 2 90.89(4)
N Ru N 3 12 180.0
N Ru N 2 12 89.11(4)
N Ru N 3 . 90.89(4)
N Ru N 2 . 90.89(4)
N Ru N 12 . 89.11(4)
N Ru N 3 11 89.11(4)
N Ru N 2 11 180.0
N Ru N 12 11 90.89(4)
N Ru N . 11 89.11(4)
N Ru N 3 10 89.11(4)
N Ru N 2 10 89.11(4)
N Ru N 12 10 90.89(4)
N Ru N . 10 180.0
N Ru N 11 10 90.89(4)
Ru N H(1) . . 110.6(16)
Ru N H(2) . . 111.8(19)
H(1) N H(2) . . 113(3)
Ru N H(3) . . 116.0(19)
H(1) N H(3) . . 97(3)
H(2) N H(3) . . 108(3)
O(1) Cl O(2) . . 109.84(4)
O(1) Cl O(2) . 2 109.84(4)
O(2) Cl O(2) . 2 109.10(4)
O(1) Cl O(2) . 3 109.84(4)
O(2) Cl O(2) . 3 109.10(4)
O(2) Cl O(2) 2 3 109.10(4)
Cl O(2) Rb . 7_544 138.82(5)
O(2) Rb O(2) 17 18_445 108.782(18)
O(2) Rb O(2) 17 5_445 180.0
O(2) Rb O(2) 18_445 5_445 71.218(18)
O(2) Rb O(2) 17 6 71.218(18)
O(2) Rb O(2) 18_445 6 180.0
O(2) Rb O(2) 5_445 6 108.782(18)
O(2) Rb O(2) 17 16_545 108.781(18)
O(2) Rb O(2) 18_445 16_545 108.781(18)
O(2) Rb O(2) 5_445 16_545 71.219(18)
O(2) Rb O(2) 6 16_545 71.219(18)
O(2) Rb O(2) 17 4_455 71.219(18)
O(2) Rb O(2) 18_445 4_455 71.219(18)
O(2) Rb O(2) 5_445 4_455 108.781(18)
O(2) Rb O(2) 6 4_455 108.781(18)
O(2) Rb O(2) 16_545 4_455 180.0
O(2) Rb Cl(1) 17 10_556 110.153(18)
O(2) Rb Cl(1) 18_445 10_556 110.153(18)
O(2) Rb Cl(1) 5_445 10_556 69.847(18)
O(2) Rb Cl(1) 6 10_556 69.847(18)
O(2) Rb Cl(1) 16_545 10_556 110.152(18)
O(2) Rb Cl(1) 4_455 10_556 69.848(18)
O(2) Rb Cl(1) 17 . 69.847(18)
O(2) Rb Cl(1) 18_445 . 69.847(18)
O(2) Rb Cl(1) 5_445 . 110.153(18)
O(2) Rb Cl(1) 6 . 110.153(18)
O(2) Rb Cl(1) 16_545 . 69.848(18)
O(2) Rb Cl(1) 4_455 . 110.152(18)
Cl(1) Rb Cl(1) 10_556 . 180.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ru N 3 2.1042(8)
Ru N 2 2.1042(8)
Ru N 12 2.1042(8)
Ru N . 2.1042(8)
Ru N 11 2.1042(8)
Ru N 10 2.1042(8)
N H(1) . 0.86(3)
N H(2) . 0.86(3)
N H(3) . 0.84(3)
Cl O(1) . 1.4406(12)
Cl O(2) . 1.4441(8)
Cl O(2) 2 1.4441(8)
Cl O(2) 3 1.4441(8)
O(2) Rb 7_544 2.9368(9)
Cl(1) Rb . 3.3920(9)
Rb O(2) 17 2.9367(9)
Rb O(2) 18_445 2.9367(9)
Rb O(2) 5_445 2.9367(9)
Rb O(2) 6 2.9367(9)
Rb O(2) 16_545 2.9368(9)
Rb O(2) 4_455 2.9368(9)
Rb Cl(1) 10_556 3.3920(9)