#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322327.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_4322327
loop_
_publ_author_name
'Zhiping Zheng'
'Thomas G. Gray'
'R. H. Holm'
_publ_section_title
;
 Synthesis and Structures of Solvated Monoclusters and Bridged Di- and
 Triclusters Based on the cubic Building Block [Re6(μ3-Se)8]2+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4888
_journal_page_last               4895
_journal_paper_doi               10.1021/ic9906050
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C16 H48 F12 O8 Re6 S8 Sb2 Se8'
_chemical_formula_weight         2845.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                100.36(3)
_cell_angle_beta                 94.52(3)
_cell_angle_gamma                95.38(3)
_cell_formula_units_Z            1
_cell_length_a                   9.337(2)
_cell_length_b                   11.578(2)
_cell_length_c                   13.498(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1422.2(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4030
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    19.128
_exptl_crystal_density_diffrn    3.322
_exptl_crystal_F_000             1268
_refine_diff_density_max         2.321
_refine_diff_density_min         -2.513
_refine_diff_density_rms         0.393
_refine_ls_extinction_coef       0.00155(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.879
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.879
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_obs          0.0490
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0787P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1287
_refine_ls_wR_factor_obs         0.1175
_reflns_number_observed          2240
_reflns_number_total             3715
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9906050_05.cif
_cod_data_source_block           zz58
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1422.4(5)
_cod_database_code               4322327
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re1 Re -0.13492(9) 0.95909(7) -0.41586(7) 0.0200(3) Uani 1 d . .
Re2 Re -0.09297(9) 1.12939(7) -0.51687(7) 0.0183(3) Uani 1 d . .
Re3 Re -0.11286(9) 0.91067(7) -0.60977(7) 0.0201(3) Uani 1 d . .
Se1 Se -0.1115(2) 1.1727(2) -0.3283(2) 0.0291(6) Uani 1 d . .
Se2 Se -0.3289(2) 0.9981(2) -0.5418(2) 0.0298(6) Uani 1 d . .
Se3 Se -0.1492(2) 0.7487(2) -0.5097(2) 0.0255(6) Uani 1 d . .
Se4 Se 0.0703(3) 0.9225(2) -0.2961(2) 0.0314(6) Uani 1 d . .
Sb Sb -0.2559(2) 0.2710(2) -0.9499(2) 0.0543(6) Uani 1 d . .
S1 S -0.2974(7) 0.9745(5) -0.2118(5) 0.036(2) Uani 1 d . .
S2 S -0.3452(6) 1.2814(5) -0.5854(5) 0.0293(14) Uani 1 d . .
S3 S -0.2310(7) 0.6879(5) -0.7877(5) 0.038(2) Uani 1 d . .
S4 S -0.1864(8) 1.5915(6) -0.2788(6) 0.053(2) Uani 1 d . .
F1 F -0.0699(23) 0.2324(22) -0.9363(21) 0.136(9) Uani 1 d . .
F2 F -0.2448(37) 0.2626(20) -1.0851(15) 0.168(13) Uani 1 d . .
F3 F -0.3349(29) 0.1116(19) -0.9754(20) 0.144(10) Uani 1 d . .
F4 F -0.2694(26) 0.2837(22) -0.8154(15) 0.130(9) Uani 1 d . .
F5 F -0.1801(27) 0.4282(16) -0.9202(23) 0.146(11) Uani 1 d . .
F6 F -0.4376(25) 0.3093(25) -0.9618(21) 0.150(10) Uani 1 d . .
O1 O -0.2974(16) 0.9055(12) -0.3215(12) 0.037(4) Uani 1 d . .
O2 O -0.1941(14) 1.2831(11) -0.5368(12) 0.030(4) Uani 1 d . .
O3 O -0.2563(18) 0.8103(12) -0.7351(12) 0.041(4) Uani 1 d . .
O4 O -0.3210(18) 1.5515(16) -0.3491(15) 0.066(6) Uani 1 d . .
C1 C -0.4721(33) 1.0097(27) -0.2028(26) 0.081(10) Uiso 1 d . .
H1A H -0.4879(33) 1.0725(27) -0.2387(26) 0.121 Uiso 1 calc R .
H1B H -0.4868(33) 1.0346(27) -0.1329(26) 0.121 Uiso 1 calc R .
H1C H -0.5388(33) 0.9415(27) -0.2317(26) 0.121 Uiso 1 calc R .
C2 C -0.3046(35) 0.8609(26) -0.1404(25) 0.079(10) Uiso 1 d . .
H2A H -0.2129(35) 0.8299(26) -0.1374(25) 0.118 Uiso 1 calc R .
H2B H -0.3785(35) 0.7990(26) -0.1719(25) 0.118 Uiso 1 calc R .
H2C H -0.3264(35) 0.8920(26) -0.0731(25) 0.118 Uiso 1 calc R .
C3 C -0.3426(26) 1.4249(18) -0.6108(18) 0.037(6) Uiso 1 d . .
H3A H -0.2862(26) 1.4316(18) -0.6664(18) 0.055 Uiso 1 calc R .
H3B H -0.3005(26) 1.4808(18) -0.5520(18) 0.055 Uiso 1 calc R .
H3C H -0.4396(26) 1.4409(18) -0.6280(18) 0.055 Uiso 1 calc R .
C4 C -0.4530(26) 1.2963(20) -0.4834(18) 0.041(6) Uiso 1 d . .
H4B H -0.4652(26) 1.2228(20) -0.4599(18) 0.062 Uiso 1 calc R .
H4C H -0.5459(26) 1.3171(20) -0.5053(18) 0.062 Uiso 1 calc R .
H4D H -0.4068(26) 1.3571(20) -0.4294(18) 0.062 Uiso 1 calc R .
C5 C -0.4152(33) 0.6192(26) -0.8174(25) 0.077(10) Uiso 1 d . .
H5A H -0.4523(33) 0.6008(26) -0.7570(25) 0.115 Uiso 1 calc R .
H5B H -0.4175(33) 0.5479(26) -0.8667(25) 0.115 Uiso 1 calc R .
H5C H -0.4737(33) 0.6725(26) -0.8442(25) 0.115 Uiso 1 calc R .
C6 C -0.1873(41) 0.7127(32) -0.9032(28) 0.108(13) Uiso 1 d . .
H6A H -0.0897(41) 0.7497(32) -0.8970(28) 0.161 Uiso 1 calc R .
H6B H -0.2518(41) 0.7635(32) -0.9276(28) 0.161 Uiso 1 calc R .
H6C H -0.1956(41) 0.6389(32) -0.9501(28) 0.161 Uiso 1 calc R .
C7 C -0.0408(25) 1.5290(20) -0.3379(19) 0.039(6) Uiso 1 d . .
H7A H -0.0217(25) 1.5648(20) -0.3950(19) 0.059 Uiso 1 calc R .
H7B H -0.0659(25) 1.4455(20) -0.3602(19) 0.059 Uiso 1 calc R .
H7C H 0.0439(25) 1.5428(20) -0.2904(19) 0.059 Uiso 1 calc R .
C8 C -0.1870(35) 1.5069(27) -0.1835(25) 0.079(10) Uiso 1 d . .
H8A H -0.2616(35) 1.5279(27) -0.1408(25) 0.119 Uiso 1 calc R .
H8B H -0.0950(35) 1.5219(27) -0.1438(25) 0.119 Uiso 1 calc R .
H8C H -0.2048(35) 1.4246(27) -0.2137(25) 0.119 Uiso 1 calc R .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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
_geom_angle_publ_flag
O1 Re1 Se2 90.6(4) . . ?
O1 Re1 Se3 89.7(4) . . ?
Se2 Re1 Se3 89.60(9) . . ?
O1 Re1 Se1 93.3(4) . . ?
Se2 Re1 Se1 90.17(9) . . ?
Se3 Re1 Se1 176.99(8) . . ?
O1 Re1 Se4 92.7(4) . . ?
Se2 Re1 Se4 176.75(9) . . ?
Se3 Re1 Se4 90.17(8) . . ?
Se1 Re1 Se4 89.89(9) . . ?
O1 Re1 Re3 137.2(4) . 2_574 ?
Se2 Re1 Re3 118.74(7) . 2_574 ?
Se3 Re1 Re3 118.60(7) . 2_574 ?
Se1 Re1 Re3 59.02(6) . 2_574 ?
Se4 Re1 Re3 58.69(6) . 2_574 ?
O1 Re1 Re2 134.4(4) . 2_574 ?
Se2 Re1 Re2 118.48(7) . 2_574 ?
Se3 Re1 Re2 58.74(6) . 2_574 ?
Se1 Re1 Re2 118.89(7) . 2_574 ?
Se4 Re1 Re2 58.79(6) . 2_574 ?
Re3 Re1 Re2 59.87(4) 2_574 2_574 ?
O1 Re1 Re3 133.0(4) . . ?
Se2 Re1 Re3 58.58(7) . . ?
Se3 Re1 Re3 58.71(6) . . ?
Se1 Re1 Re3 118.75(7) . . ?
Se4 Re1 Re3 118.69(7) . . ?
Re3 Re1 Re3 89.71(5) 2_574 . ?
Re2 Re1 Re3 59.91(4) 2_574 . ?
O1 Re1 Re2 135.7(4) . . ?
Se2 Re1 Re2 58.88(6) . . ?
Se3 Re1 Re2 118.49(7) . . ?
Se1 Re1 Re2 58.97(6) . . ?
Se4 Re1 Re2 118.55(7) . . ?
Re3 Re1 Re2 59.87(4) 2_574 . ?
Re2 Re1 Re2 89.80(4) 2_574 . ?
Re3 Re1 Re2 59.79(4) . . ?
O2 Re2 Se3 89.4(4) . 2_574 ?
O2 Re2 Se4 90.9(4) . 2_574 ?
Se3 Re2 Se4 90.48(9) 2_574 2_574 ?
O2 Re2 Se2 93.6(4) . . ?
Se3 Re2 Se2 177.00(8) 2_574 . ?
Se4 Re2 Se2 89.61(9) 2_574 . ?
O2 Re2 Se1 91.7(4) . . ?
Se3 Re2 Se1 89.83(9) 2_574 . ?
Se4 Re2 Se1 177.40(8) 2_574 . ?
Se2 Re2 Se1 89.95(9) . . ?
O2 Re2 Re3 136.1(4) . . ?
Se3 Re2 Re3 119.04(7) 2_574 . ?
Se4 Re2 Re3 58.83(6) 2_574 . ?
Se2 Re2 Re3 58.60(6) . . ?
Se1 Re2 Re3 118.85(7) . . ?
O2 Re2 Re3 134.0(4) . 2_574 ?
Se3 Re2 Re3 58.84(6) 2_574 2_574 ?
Se4 Re2 Re3 119.10(7) 2_574 2_574 ?
Se2 Re2 Re3 118.62(7) . 2_574 ?
Se1 Re2 Re3 59.01(6) . 2_574 ?
Re3 Re2 Re3 89.90(5) . 2_574 ?
O2 Re2 Re1 133.2(4) . 2_574 ?
Se3 Re2 Re1 59.00(6) 2_574 2_574 ?
Se4 Re2 Re1 59.04(7) 2_574 2_574 ?
Se2 Re2 Re1 118.64(7) . 2_574 ?
Se1 Re2 Re1 119.07(7) . 2_574 ?
Re3 Re2 Re1 60.05(4) . 2_574 ?
Re3 Re2 Re1 60.07(4) 2_574 2_574 ?
O2 Re2 Re1 136.6(4) . . ?
Se3 Re2 Re1 118.80(7) 2_574 . ?
Se4 Re2 Re1 118.86(7) 2_574 . ?
Se2 Re2 Re1 58.67(6) . . ?
Se1 Re2 Re1 58.82(6) . . ?
Re3 Re2 Re1 60.03(3) . . ?
Re3 Re2 Re1 59.96(4) 2_574 . ?
Re1 Re2 Re1 90.20(4) 2_574 . ?
O3 Re3 Se2 87.8(4) . . ?
O3 Re3 Se4 91.1(4) . 2_574 ?
Se2 Re3 Se4 90.02(8) . 2_574 ?
O3 Re3 Se3 91.2(4) . . ?
Se2 Re3 Se3 89.95(8) . . ?
Se4 Re3 Se3 177.73(9) 2_574 . ?
O3 Re3 Se1 94.6(4) . 2_574 ?
Se2 Re3 Se1 177.57(9) . 2_574 ?
Se4 Re3 Se1 90.07(9) 2_574 2_574 ?
Se3 Re3 Se1 89.87(8) . 2_574 ?
O3 Re3 Re2 132.5(4) . . ?
Se2 Re3 Re2 59.12(6) . . ?
Se4 Re3 Re2 58.99(6) 2_574 . ?
Se3 Re3 Re2 119.16(7) . . ?
Se1 Re3 Re2 118.98(7) 2_574 . ?
O3 Re3 Re2 137.3(4) . 2_574 ?
Se2 Re3 Re2 118.90(7) . 2_574 ?
Se4 Re3 Re2 119.26(7) 2_574 2_574 ?
Se3 Re3 Re2 58.87(6) . 2_574 ?
Se1 Re3 Re2 59.05(7) 2_574 2_574 ?
Re2 Re3 Re2 90.10(5) . 2_574 ?
O3 Re3 Re1 137.2(5) . 2_574 ?
Se2 Re3 Re1 119.19(7) . 2_574 ?
Se4 Re3 Re1 59.10(7) 2_574 2_574 ?
Se3 Re3 Re1 119.04(7) . 2_574 ?
Se1 Re3 Re1 58.91(6) 2_574 2_574 ?
Re2 Re3 Re1 60.08(4) . 2_574 ?
Re2 Re3 Re1 60.17(4) 2_574 2_574 ?
O3 Re3 Re1 132.4(5) . . ?
Se2 Re3 Re1 58.88(7) . . ?
Se4 Re3 Re1 119.17(7) 2_574 . ?
Se3 Re3 Re1 58.99(6) . . ?
Se1 Re3 Re1 119.06(7) 2_574 . ?
Re2 Re3 Re1 60.18(4) . . ?
Re2 Re3 Re1 60.02(4) 2_574 . ?
Re1 Re3 Re1 90.29(5) 2_574 . ?
Re1 Se1 Re3 62.07(6) . 2_574 ?
Re1 Se1 Re2 62.20(7) . . ?
Re3 Se1 Re2 61.95(7) 2_574 . ?
Re3 Se2 Re1 62.54(6) . . ?
Re3 Se2 Re2 62.29(6) . . ?
Re1 Se2 Re2 62.45(6) . . ?
Re3 Se3 Re2 62.28(6) . 2_574 ?
Re3 Se3 Re1 62.30(6) . . ?
Re2 Se3 Re1 62.26(6) 2_574 . ?
Re3 Se4 Re2 62.18(7) 2_574 2_574 ?
Re3 Se4 Re1 62.21(7) 2_574 . ?
Re2 Se4 Re1 62.17(7) 2_574 . ?
F6 Sb F4 87.9(12) . . ?
F6 Sb F2 90.8(14) . . ?
F4 Sb F2 178.2(11) . . ?
F6 Sb F1 179.4(14) . . ?
F4 Sb F1 91.5(11) . . ?
F2 Sb F1 89.7(14) . . ?
F6 Sb F5 92.0(12) . . ?
F4 Sb F5 86.3(12) . . ?
F2 Sb F5 92.4(12) . . ?
F1 Sb F5 87.8(11) . . ?
F6 Sb F3 87.6(12) . . ?
F4 Sb F3 91.7(11) . . ?
F2 Sb F3 89.5(11) . . ?
F1 Sb F3 92.7(12) . . ?
F5 Sb F3 178.0(12) . . ?
O1 S1 C1 105.0(13) . . ?
O1 S1 C2 102.6(12) . . ?
C1 S1 C2 98.0(15) . . ?
O2 S2 C3 101.7(10) . . ?
O2 S2 C4 104.5(11) . . ?
C3 S2 C4 99.0(11) . . ?
O3 S3 C6 101.9(14) . . ?
O3 S3 C5 100.6(12) . . ?
C6 S3 C5 101.7(17) . . ?
O4 S4 C8 108.0(14) . . ?
O4 S4 C7 107.7(11) . . ?
C8 S4 C7 95.7(13) . . ?
S1 O1 Re1 119.6(8) . . ?
S2 O2 Re2 124.8(8) . . ?
S3 O3 Re3 122.5(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O1 2.173(14) . ?
Re1 Se2 2.514(3) . ?
Re1 Se3 2.522(2) . ?
Re1 Se1 2.523(2) . ?
Re1 Se4 2.525(3) . ?
Re1 Re3 2.6035(14) 2_574 ?
Re1 Re2 2.6040(13) 2_574 ?
Re1 Re3 2.6052(14) . ?
Re1 Re2 2.6090(13) . ?
Re2 O2 2.140(13) . ?
Re2 Se3 2.515(2) 2_574 ?
Re2 Se4 2.518(3) 2_574 ?
Re2 Se2 2.519(3) . ?
Re2 Se1 2.527(3) . ?
Re2 Re3 2.5986(14) . ?
Re2 Re3 2.6010(14) 2_574 ?
Re2 Re1 2.6040(13) 2_574 ?
Re3 O3 2.156(15) . ?
Re3 Se2 2.505(2) . ?
Re3 Se4 2.514(3) 2_574 ?
Re3 Se3 2.514(2) . ?
Re3 Se1 2.526(2) 2_574 ?
Re3 Re2 2.6010(14) 2_574 ?
Re3 Re1 2.6034(14) 2_574 ?
Se1 Re3 2.526(2) 2_574 ?
Se3 Re2 2.515(2) 2_574 ?
Se4 Re3 2.514(3) 2_574 ?
Se4 Re2 2.518(3) 2_574 ?
Sb F6 1.80(2) . ?
Sb F4 1.81(2) . ?
Sb F2 1.82(2) . ?
Sb F1 1.84(2) . ?
Sb F5 1.85(2) . ?
Sb F3 1.88(2) . ?
S1 O1 1.55(2) . ?
S1 C1 1.73(3) . ?
S1 C2 1.76(3) . ?
S2 O2 1.505(14) . ?
S2 C3 1.76(2) . ?
S2 C4 1.76(2) . ?
S3 O3 1.515(15) . ?
S3 C6 1.71(4) . ?
S3 C5 1.81(3) . ?
S4 O4 1.50(2) . ?
S4 C8 1.75(3) . ?
S4 C7 1.78(2) . ?
