#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322326.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_4322326
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            'C18 H42 F12 N6 O6 Re6 Sb2 Se8'
_chemical_formula_weight         2658.96
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.550(2)
_cell_length_b                   12.550(2)
_cell_length_c                   27.039(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3688.2(11)
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            1780
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    21.791
_exptl_crystal_density_diffrn    3.592
_exptl_crystal_F_000             3516
_refine_diff_density_max         1.569
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       0.00015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.569
_refine_ls_goodness_of_fit_obs   0.618
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.569
_refine_ls_restrained_S_obs      0.618
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_obs          0.0337
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1009
_refine_ls_wR_factor_obs         0.0818
_reflns_number_observed          634
_reflns_number_total             1077
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9906050_04.cif
_cod_data_source_block           zz57a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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        3688.0(10)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4322326
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_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 0.53879(6) 0.31546(6) 0.29397(2) 0.0252(3) Uani 1 d . .
Se1 Se 0.4202(2) 0.2989(2) 0.37165(6) 0.0367(6) Uani 1 d . .
Se2 Se 0.6667 0.3333 0.21900(11) 0.0313(8) Uani 1 d S .
Sb Sb 0.6667 0.3333 -0.06111(10) 0.0661(9) Uani 1 d S .
F1 F 0.7697(24) 0.3080(29) -0.1001(8) 0.197(12) Uani 1 d . .
F2 F 0.6470(38) 0.2101(29) -0.0205(10) 0.279(17) Uani 1 d . .
O O 0.3948(11) 0.2976(11) 0.2462(4) 0.038(3) Uani 1 d . .
N N 0.2101(13) 0.2632(14) 0.2265(5) 0.038(4) Uani 1 d . .
C1 C 0.2850(18) 0.2599(17) 0.2573(7) 0.041(5) Uani 1 d . .
H1A H 0.2573(18) 0.2287(17) 0.2888(7) 0.180(144) Uiso 1 calc R .
C2 C 0.2466(21) 0.3092(24) 0.1763(8) 0.074(7) Uani 1 d . .
H2A H 0.1774(21) 0.3042(24) 0.1590(8) 0.112 Uiso 1 calc R .
H2B H 0.2746(21) 0.2604(24) 0.1594(8) 0.112 Uiso 1 calc R .
H2C H 0.3118(21) 0.3934(24) 0.1773(8) 0.112 Uiso 1 calc R .
C3 C 0.0814(16) 0.2223(23) 0.2377(8) 0.070(8) Uani 1 d . .
H3A H 0.0427(16) 0.2332(23) 0.2091(8) 0.105 Uiso 1 calc R .
H3B H 0.0772(16) 0.2698(23) 0.2647(8) 0.105 Uiso 1 calc R .
H3C H 0.0399(16) 0.1369(23) 0.2467(8) 0.105 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'
N N 0.0061 0.0033 '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'
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
O Re1 Se1 92.1(3) . 18_545 ?
O Re1 Se1 90.7(3) . 17 ?
Se1 Re1 Se1 177.21(6) 18_545 17 ?
O Re1 Se1 93.5(3) . . ?
Se1 Re1 Se1 90.16(5) 18_545 . ?
Se1 Re1 Se1 90.15(5) 17 . ?
O Re1 Se2 89.5(3) . . ?
Se1 Re1 Se2 89.78(5) 18_545 . ?
Se1 Re1 Se2 89.77(5) 17 . ?
Se1 Re1 Se2 177.03(6) . . ?
O Re1 Re1 136.8(3) . 18_545 ?
Se1 Re1 Re1 58.99(4) 18_545 18_545 ?
Se1 Re1 Re1 118.98(5) 17 18_545 ?
Se1 Re1 Re1 58.68(5) . 18_545 ?
Se2 Re1 Re1 118.91(4) . 18_545 ?
O Re1 Re1 135.8(3) . 17 ?
Se1 Re1 Re1 118.98(5) 18_545 17 ?
Se1 Re1 Re1 58.98(4) 17 17 ?
Se1 Re1 Re1 58.66(5) . 17 ?
Se2 Re1 Re1 118.91(4) . 17 ?
Re1 Re1 Re1 60.01(3) 18_545 17 ?
O Re1 Re1 133.2(3) . 3_665 ?
Se1 Re1 Re1 118.77(6) 18_545 3_665 ?
Se1 Re1 Re1 58.75(6) 17 3_665 ?
Se1 Re1 Re1 118.65(5) . 3_665 ?
Se2 Re1 Re1 58.92(3) . 3_665 ?
Re1 Re1 Re1 90.0 18_545 3_665 ?
Re1 Re1 Re1 60.00(2) 17 3_665 ?
O Re1 Re1 134.2(3) . 2_655 ?
Se1 Re1 Re1 58.77(6) 18_545 2_655 ?
Se1 Re1 Re1 118.75(6) 17 2_655 ?
Se1 Re1 Re1 118.67(5) . 2_655 ?
Se2 Re1 Re1 58.92(3) . 2_655 ?
Re1 Re1 Re1 60.00(2) 18_545 2_655 ?
Re1 Re1 Re1 90.0 17 2_655 ?
Re1 Re1 Re1 60.0 3_665 2_655 ?
Re1 Se1 Re1 62.47(5) 17 18_545 ?
Re1 Se1 Re1 62.35(5) 17 . ?
Re1 Se1 Re1 62.35(5) 18_545 . ?
Re1 Se2 Re1 62.17(7) 3_665 2_655 ?
Re1 Se2 Re1 62.16(7) 3_665 . ?
Re1 Se2 Re1 62.17(7) 2_655 . ?
F2 Sb F2 87.0(15) 2_655 . ?
F2 Sb F2 87.0(15) 2_655 3_665 ?
F2 Sb F2 87.0(15) . 3_665 ?
F2 Sb F1 92.9(15) 2_655 . ?
F2 Sb F1 90.4(13) . . ?
F2 Sb F1 177.5(15) 3_665 . ?
F2 Sb F1 177.5(15) 2_655 3_665 ?
F2 Sb F1 92.9(15) . 3_665 ?
F2 Sb F1 90.4(13) 3_665 3_665 ?
F1 Sb F1 89.6(10) . 3_665 ?
F2 Sb F1 90.4(13) 2_655 2_655 ?
F2 Sb F1 177.5(16) . 2_655 ?
F2 Sb F1 92.9(15) 3_665 2_655 ?
F1 Sb F1 89.6(10) . 2_655 ?
F1 Sb F1 89.6(10) 3_665 2_655 ?
C1 O Re1 127.6(11) . . ?
C1 N C2 122.2(16) . . ?
C1 N C3 123.9(16) . . ?
C2 N C3 113.9(15) . . ?
O C1 N 121.6(17) . . ?
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 O 2.139(11) . ?
Re1 Se1 2.514(2) 18_545 ?
Re1 Se1 2.514(2) 17 ?
Re1 Se1 2.522(2) . ?
Re1 Se2 2.525(2) . ?
Re1 Re1 2.6069(11) 18_545 ?
Re1 Re1 2.6069(11) 17 ?
Re1 Re1 2.6072(11) 3_665 ?
Re1 Re1 2.6072(11) 2_655 ?
Se1 Re1 2.514(2) 17 ?
Se1 Re1 2.514(2) 18_545 ?
Se2 Re1 2.525(2) 3_665 ?
Se2 Re1 2.525(2) 2_655 ?
Sb F2 1.81(2) 2_655 ?
Sb F2 1.81(2) . ?
Sb F2 1.81(2) 3_665 ?
Sb F1 1.82(2) . ?
Sb F1 1.82(2) 3_665 ?
Sb F1 1.82(2) 2_655 ?
O C1 1.25(2) . ?
N C1 1.27(2) . ?
N C2 1.46(2) . ?
N C3 1.46(2) . ?
