#------------------------------------------------------------------------------
#$Date: 2017-01-27 12:59:36 +0200 (Fri, 27 Jan 2017) $
#$Revision: 191017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/49/2004943.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_2004943
loop_
_publ_author_name
'Blake, A. J.'
'Radek, C.'
'Schröder, M.'
_publ_section_title
;Tris(1,4,7,10-tetraoxa-13,16-dithiacyclooctadecane-S,S')ruthenium(II)
 Bis(hexafluorophosphate)--Water--Methanol (1/2/1)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1401
_journal_page_last               1403
_journal_paper_doi               10.1107/S0108270196001497
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac
'[Ru (C12 H24 O4 S2)3](P F6)2, 2H2 O1, C1 H4 O1'
_chemical_formula_moiety
'C36 H72 O12 S6 Ru 2+,2(P F6 -),2(H2 O),C H3 O H'
_chemical_formula_sum            'C37 H80 F12 O15 P2 Ru S6'
_chemical_formula_weight         1348.19
_chemical_name_systematic
;
Tris(1,4,7,10-tetraoxa-13,16-dithiacyclooctadecane)ruthenium(II)
bis(hexafluorophosphate) dihydrate methanol solvate
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.629(2)
_cell_length_b                   18.629(2)
_cell_length_c                   29.863(5)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     8975(2)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1990a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1990b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELX76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       'learnt-profile (Clegg, 1981)'
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3380
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_meas      1.49
_exptl_crystal_density_method    flotation
_exptl_crystal_description       tablet
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_hydrogen_treatment
;
H atoms riding with U~iso~(H) = 1.2U~eq~(C); water and methanol
H atoms not located
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.251
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_obs          0.0361
_refine_ls_shift/esd_max         0.30
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.060P)^2^ + 42.41P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1275
_refine_ls_wR_factor_obs         0.1002
_reflns_number_observed          2270
_reflns_number_total             2608
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab1354.cif
_cod_data_source_block           rusoox
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-01-27
;
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               2004943
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_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
_atom_site_attached_hydrogens
Ru 1 0 0 .212934(15) .0246(2) Uani d S Ru 0
S1 1 -.03570(6) .08846(6) .25311(3) .0310(3) Uani d . S 0
C2 1 -0.1241(2) .0783(2) .22131(12) .0350(9) Uani d . C 0
H2A 1 -0.1563(2) .0956(2) .24036(12) .042 Uiso calc R H 0
H2B 1 -0.1036(2) .1158(2) .19508(12) .042 Uiso calc R H 0
C3 1 -0.1797(2) -.0089(2) .20558(13) .0352(9) Uani d . C 0
H3A 1 -0.2260(2) -.0115(2) .18801(13) .042 Uiso calc R H 0
H3B 1 -0.2034(2) -.0459(2) .23180(13) .042 Uiso calc R H 0
S4 1 -0.12261(5) -.04416(5) .17105(3) .0284(3) Uani d . S 0
C5 1 -0.1080(2) .0156(2) .11998(11) .0304(8) Uani d . C 0
H5A 1 -0.1003(2) .0706(2) .12793(11) .036 Uiso calc R H 0
H5B 1 -.0573(2) .0244(2) .10445(11) .036 Uiso calc R H 0
C6 1 -0.1817(2) -.0284(2) .08861(12) .0341(9) Uani d . C 0
H6A 1 -0.1685(2) .0024(2) .05999(12) .041 Uiso calc R H 0
H6B 1 -0.1909(2) -.0845(2) .08209(12) .041 Uiso calc R H 0
O7 1 -0.25629(15) -.0360(2) .10615(8) .0344(6) Uani d . O 0
C8 1 -0.2629(2) .0368(2) .09855(13) .0388(9) Uani d . C 0
H8A 1 -0.2717(2) .0420(2) .06631(13) .047 Uiso calc R H 0
H8B 1 -0.2112(2) .0869(2) .10801(13) .047 Uiso calc R H 0
C9 1 -0.3345(3) .0285(3) .12513(13) .0429(10) Uani d . C 0
H9A 1 -0.3493(3) .0701(3) .11508(13) .051 Uiso calc R H 0
H9B 1 -0.3833(3) -.0274(3) .12084(13) .051 Uiso calc R H 0
O10 1 -0.3113(2) .0412(2) .17101(9) .0463(7) Uani d . O 0
C11 1 -0.3774(3) .0283(3) .19959(15) .0492(11) Uani d . C 0
H11A 1 -0.4263(3) -.0266(3) .19336(15) .059 Uiso calc R H 0
H11B 1 -0.3929(3) .0711(3) .19372(15) .059 Uiso calc R H 0
C12 1 -0.3526(3) .0325(3) .24726(14) .0489(11) Uani d . C 0
H12A 1 -0.4013(3) .0164(3) .26675(14) .059 Uiso calc R H 0
H12B 1 -0.3328(3) -.0072(3) .25246(14) .059 Uiso calc R H 0
O13 1 -0.2887(2) .1141(2) .25859(9) .0466(7) Uani d . O 0
C14 1 -0.2766(3) .1267(3) .30565(13) .0454(10) Uani d . C 0
H14A 1 -0.3316(3) .1005(3) .32030(13) .054 Uiso calc R H 0
H14B 1 -0.2490(3) .1869(3) .31168(13) .054 Uiso calc R H 0
C15 1 -0.2263(3) .0931(3) .32697(14) .0441(10) Uani d . C 0
H15A 1 -0.2328(3) .0917(3) .35992(14) .053 Uiso calc R H 0
H15B 1 -0.2461(3) .0359(3) .31638(14) .053 Uiso calc R H 0
O16 1 -0.1412(2) .1448(2) .31542(9) .0410(7) Uani d . O 0
C17 1 -.0892(3) .1173(3) .33456(14) .0450(10) Uani d . C 0
H17A 1 -0.1097(3) .0956(3) .36496(14) .054 Uiso calc R H 0
H17B 1 -.0325(3) .1655(3) .33770(14) .054 Uiso calc R H 0
C18 1 -.0846(3) .0502(3) .30735(12) .0373(9) Uani d . C 0
H18A 1 -0.1413(3) .0030(3) .30280(12) .045 Uiso calc R H 0
H18B 1 -.0528(3) .0299(3) .32439(12) .045 Uiso calc R H 0
P1 1 0 0 0 .0292(5) Uani d S P 0
F11 1 .00286(14) .07149(13) .03095(7) .0409(5) Uani d . F 0
P2 1 0 .5 0 .0540(5) Uani d S P 0
F21 1 .0927(2) .5565(2) .01702(12) .0826(9) Uani d . F 0
F22 1 -.0266(2) .4535(2) .04606(11) .0844(10) Uani d . F 0
F23 1 -.0216(2) .5671(2) .01779(13) .0868(11) Uani d . F 0
O1W 1 .3333 .6667 .0703(4) .158(4) Uiso d S O 2
O2W .33 .5770(13) .8251(13) .1388(7) .150(7) Uiso d P O 2
O1M .33 .4050(12) .8616(12) .1196(6) .135(6) Uiso d P O 1
C2M .33 .4388(15) .8224(15) .1073(8) .110(7) Uiso d P C 3
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
S4 Ru S4 2 3 94.55(3) n
S4 Ru S4 2 . 94.55(3) y
S4 Ru S4 3 . 94.55(3) n
S4 Ru S1 2 . 175.66(3) y
S4 Ru S1 3 . 81.35(3) n
S4 Ru S1 . . 87.24(3) y
S4 Ru S1 2 3 81.36(3) n
S4 Ru S1 3 3 87.25(3) n
S4 Ru S1 . 3 175.66(3) n
S1 Ru S1 . 3 96.94(3) n
S4 Ru S1 2 2 87.24(3) n
S4 Ru S1 3 2 175.66(3) n
S4 Ru S1 . 2 81.36(3) y
S1 Ru S1 . 2 96.94(3) y
S1 Ru S1 3 2 96.93(3) n
C18 S1 C2 . . 100.0(2) y
C18 S1 Ru . . 115.80(13) n
C2 S1 Ru . . 102.45(12) n
C3 C2 S1 . . 111.9(3) y
C2 C3 S4 . . 110.9(3) y
C3 S4 C5 . . 100.8(2) y
C3 S4 Ru . . 102.22(13) n
C5 S4 Ru . . 113.98(12) n
C6 C5 S4 . . 111.5(2) y
O7 C6 C5 . . 113.6(3) y
C6 O7 C8 . . 112.8(3) y
O7 C8 C9 . . 108.2(3) y
O10 C9 C8 . . 108.3(3) y
C11 O10 C9 . . 112.7(3) y
O10 C11 C12 . . 110.3(4) y
O13 C12 C11 . . 110.8(3) y
C14 O13 C12 . . 112.9(3) y
O13 C14 C15 . . 115.4(3) y
O16 C15 C14 . . 109.3(3) y
C17 O16 C15 . . 112.8(3) y
O16 C17 C18 . . 114.0(3) y
C17 C18 S1 . . 112.0(3) y
F11 P1 F11 . 10 180.0 n
F11 P1 F11 . 2 89.96(11) n
F11 P1 F11 10 2 90.04(11) n
F11 P1 F11 . 12 90.04(11) n
F11 P1 F11 10 12 89.96(11) n
F11 P1 F11 2 12 90.04(11) n
F11 P1 F11 . 3 89.96(11) n
F11 P1 F11 10 3 90.04(11) n
F11 P1 F11 2 3 89.96(11) n
F11 P1 F11 12 3 180.0 n
F11 P1 F11 . 11 90.04(11) n
F11 P1 F11 10 11 89.96(11) n
F11 P1 F11 2 11 180.0 n
F11 P1 F11 12 11 89.96(11) n
F11 P1 F11 3 11 90.04(11) n
F22 P2 F22 10_565 . 180.0 n
F22 P2 F23 10_565 10_565 90.4(2) n
F22 P2 F23 . 10_565 89.6(2) n
F22 P2 F23 10_565 . 89.6(2) n
F22 P2 F23 . . 90.4(2) n
F23 P2 F23 10_565 . 180.0 n
F22 P2 F21 10_565 . 88.6(2) n
F22 P2 F21 . . 91.4(2) n
F23 P2 F21 10_565 . 90.5(2) n
F23 P2 F21 . . 89.5(2) n
F22 P2 F21 10_565 10_565 91.4(2) n
F22 P2 F21 . 10_565 88.6(2) n
F23 P2 F21 10_565 10_565 89.5(2) n
F23 P2 F21 . 10_565 90.5(2) n
F21 P2 F21 . 10_565 180.0 n
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
Ru S4 2 2.3620(9) n
Ru S4 3 2.3620(9) n
Ru S1 . 2.3859(9) y
Ru S4 . 2.3620(9) y
Ru S1 3 2.3859(9) n
Ru S1 2 2.3859(9) n
S1 C18 . 1.820(4) y
S1 C2 . 1.827(4) y
C2 C3 . 1.500(6) y
C3 S4 . 1.824(4) y
S4 C5 . 1.827(3) y
C5 C6 . 1.520(5) y
C6 O7 . 1.424(4) y
O7 C8 . 1.440(5) y
C8 C9 . 1.492(6) y
C9 O10 . 1.421(5) y
O10 C11 . 1.416(5) y
C11 C12 . 1.487(6) y
C12 O13 . 1.426(5) y
O13 C14 . 1.424(5) y
C14 C15 . 1.503(6) y
C15 O16 . 1.425(5) y
O16 C17 . 1.423(5) y
C17 C18 . 1.528(6) y
P1 F11 . 1.600(2) n
P1 F11 10 1.600(2) n
P1 F11 2 1.600(2) n
P1 F11 12 1.600(2) n
P1 F11 3 1.600(2) n
P1 F11 11 1.600(2) n
P2 F22 10_565 1.568(3) n
P2 F22 . 1.568(3) n
P2 F23 10_565 1.584(3) n
P2 F23 . 1.584(3) n
P2 F21 . 1.591(3) n
P2 F21 10_565 1.591(3) n
O1M C2M . 1.24(3) n
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
_geom_torsion_publ_flag
C18 S1 C2 C3 -80.6(3) y
S1 C2 C3 S4 -58.0(3) y
C2 C3 S4 C5 -72.4(3) y
C3 S4 C5 C6 -86.3(3) y
S4 C5 C6 O7 65.4(4) y
C5 C6 O7 C8 84.1(4) y
C6 O7 C8 C9 -169.9(3) y
O7 C8 C9 O10 73.6(4) y
C8 C9 O10 C11 -175.4(3) y
C9 O10 C11 C12 173.2(3) y
O10 C11 C12 O13 66.2(5) y
C11 C12 O13 C14 165.8(3) y
C12 O13 C14 C15 79.8(4) y
O13 C14 C15 O16 73.7(5) y
C14 C15 O16 C17 179.7(3) y
C15 O16 C17 C18 84.3(4) y
O16 C17 C18 S1 65.4(4) y
C2 S1 C18 C17 -82.4(3) y
