#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:49:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179492 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/89/4338923.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4338923
loop_
_publ_author_name
'Brylev, Konstantin A.'
'Mironov, Yuri V.'
'Yarovoi, Spartak S.'
'Naumov, Nikolai G.'
'Fedorov, Vladimir E.'
'Kim, Sung-Jin'
'Kitamura, Noboru'
'Kuwahara, Yusuke'
'Yamada, Konatsu'
'Ishizaka, Shoji'
'Sasaki, Yoichi'
_publ_section_title
;
 A family of octahedral rhenium cluster complexes [Re6Q8(H2O)n(OH)6-n]n-4
 (Q=S, Se; n=0-6): structural and pH-dependent spectroscopic studies.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7414
_journal_page_last               7422
_journal_paper_doi               10.1021/ic7005265
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '[Re6S8(H2O)4(OH)2].12H2O'
_chemical_formula_sum            'H34 O18 Re6 S8'
_chemical_formula_weight         1695.95
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                   14.9959(13)
_cell_length_b                   14.9959(13)
_cell_length_c                   10.9403(19)
_cell_measurement_temperature    173(2)
_cell_volume                     2130.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'φ scans'
_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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4477
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    26.114
_exptl_absorpt_correction_T_max  0.3033
_exptl_absorpt_correction_T_min  0.2021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.00010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0204
_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)+(0.0278P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0554
_reflns_number_gt                594
_reflns_number_total             650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7005265-file003.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      R-3m
_cod_database_code               4338923
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'-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+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-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+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Re1 Re 0.057379(10) 0.942621(10) 0.40344(2) 0.01403(14) Uani 1 2 d S
S1 S 0.0000 1.0000 0.2304(3) 0.0182(6) Uani 1 6 d S
S2 S 0.21407(13) 1.10704(7) 0.41121(16) 0.0200(4) Uani 1 2 d S
O1 O 0.12241(18) 0.87759(18) 0.2869(4) 0.0245(11) Uani 1 2 d S
O1W O 0.2377(4) 1.2116(4) 0.1196(4) 0.0525(13) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.01657(16) 0.01657(16) 0.01036(19) -0.00034(5) 0.00034(5) 0.00935(12)
S1 0.0208(9) 0.0208(9) 0.0128(14) 0.000 0.000 0.0104(4)
S2 0.0151(8) 0.0248(7) 0.0169(9) 0.0012(3) 0.0025(7) 0.0076(4)
O1 0.031(2) 0.031(2) 0.019(3) -0.0031(11) 0.0031(11) 0.021(2)
O1W 0.060(3) 0.077(3) 0.034(3) 0.012(2) 0.011(2) 0.044(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Re1 Re1 Re1 59.890(16) 21_666 20_456
Re1 Re1 Re1 60.0 3_465 2_675
Re1 Re1 Re1 60.055(8) 2_675 21_666
Re1 Re1 Re1 60.055(8) 3_465 20_456
Re1 Re1 Re1 90.0 2_675 20_456
Re1 Re1 Re1 90.0 3_465 21_666
S1 Re1 Re1 57.61(4) . 2_675
S1 Re1 Re1 57.61(4) . 3_465
S1 Re1 Re1 117.63(4) . 20_456
S1 Re1 Re1 117.63(4) . 21_666
S1 Re1 S2 90.11(3) . .
S1 Re1 S2 90.11(3) . 3_465
S2 Re1 Re1 57.37(4) . 21_666
S2 Re1 Re1 57.37(4) 3_465 20_456
S2 Re1 Re1 57.64(2) . 2_675
S2 Re1 Re1 57.64(2) 3_465 3_465
S2 Re1 Re1 57.67(4) 20_456 20_456
S2 Re1 Re1 57.67(4) 20_456 21_666
S2 Re1 Re1 117.23(4) . 20_456
S2 Re1 Re1 117.23(4) 3_465 21_666
S2 Re1 Re1 117.60(2) . 3_465
S2 Re1 Re1 117.60(2) 3_465 2_675
S2 Re1 Re1 117.70(3) 20_456 2_675
S2 Re1 Re1 117.70(3) 20_456 3_465
S2 Re1 S1 174.25(6) 20_456 .
S2 Re1 S2 89.57(3) 20_456 .
S2 Re1 S2 89.57(3) 20_456 3_465
S2 Re1 S2 173.75(6) . 3_465
O1 Re1 Re1 136.25(9) . 20_456
O1 Re1 Re1 136.25(9) . 21_666
O1 Re1 Re1 133.73(10) . 2_675
O1 Re1 Re1 133.73(10) . 3_465
O1 Re1 S1 91.17(14) . .
O1 Re1 S2 93.12(3) . .
O1 Re1 S2 93.12(3) . 3_465
O1 Re1 S2 94.59(14) . 20_456
Re1 S1 Re1 64.78(7) 2_675 .
Re1 S1 Re1 64.78(7) 2_675 3_465
Re1 S1 Re1 64.78(7) 3_465 .
Re1 S2 Re1 64.72(4) . 2_675
Re1 S2 Re1 64.97(4) 21_666 .
Re1 S2 Re1 64.97(4) 21_666 2_675
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 Re1 2.5813(5) 2_675
Re1 Re1 2.5813(5) 3_465
Re1 Re1 2.5856(6) 20_456
Re1 Re1 2.5856(6) 21_666
Re1 S1 2.409(2) .
Re1 S2 2.4033(17) 20_456
Re1 S2 2.4112(15) .
Re1 S2 2.4112(15) 3_465
Re1 O1 2.116(5) .
S1 Re1 2.409(2) 2_675
S1 Re1 2.409(2) 3_465
S2 Re1 2.4112(14) 2_675
S2 Re1 2.4033(17) 21_666
