#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:47:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179306 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/03/4320353.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_4320353
loop_
_publ_author_name
'Yuri V. Mironov'
'Michael A. Pell'
'Thomas E. Albrecht-Schmitt'
'James A. Ibers'
_publ_section_title
;
 The Mixed Polychalcogenorhenate(IV) Anions [Re4Q4(S3)4(S4)2]4- (Q = Se,
 Te): Syntheses and Crystal Structures of
 [NMe4]5[Me2NH2]3[Re4Se4(S3)4(S4)2]2.2.25H2O and
 [NH4]4[Re4Te4(S3)4(S4)2].8H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5472
_journal_page_last               5474
_journal_paper_doi               10.1021/ic010434a
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'H32 N4 O8 Re4 S20 Te4'
_chemical_formula_weight         2112.7
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6463(7)
_cell_length_b                   16.2348(9)
_cell_length_c                   19.8038(11)
_cell_measurement_temperature    153(2)
_cell_volume                     4065.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'standard-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23340
_diffrn_reflns_theta_full        28.78
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    15.744
_exptl_absorpt_correction_T_max  0.32673
_exptl_absorpt_correction_T_min  0.17255
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sq.prizm.
_exptl_crystal_F_000             3816
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.112
_refine_diff_density_max         2.593
_refine_diff_density_min         -2.403
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0265
_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)+(0.0300P)²+70.3159P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                2525
_reflns_number_total             2736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010434a_2.cif
_cod_data_source_block           sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorombic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320353
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, 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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.11592(2) 0.356804(17) 0.2500 0.01778(8) Uani 1 2 d S . .
Re2 Re 0.0000 0.236533(18) 0.323644(16) 0.02142(8) Uani 1 2 d S . .
Te1 Te 0.0000 0.39404(3) 0.35413(2) 0.02121(11) Uani 1 2 d S . .
Te2 Te 0.16459(4) 0.19915(3) 0.2500 0.02554(12) Uani 1 2 d S . .
S1 S 0.0000 0.09019(15) 0.35928(15) 0.0494(7) Uani 1 2 d S . .
S2 S 0.0501(2) 0.00854(18) 0.2908(2) 0.0401(8) Uani 0.50 1 d P . .
S3 S 0.17277(14) 0.50325(11) 0.2500 0.0229(4) Uani 1 2 d S . .
S4 S 0.0612(2) 0.58306(16) 0.21535(15) 0.0262(5) Uani 0.50 1 d P . .
S5 S 0.26797(11) 0.36255(9) 0.33189(8) 0.0309(3) Uani 1 1 d . . .
S6B S 0.2032(2) 0.33342(19) 0.43155(14) 0.0293(6) Uani 0.50 1 d P . .
S6A S 0.2828(2) 0.25636(19) 0.38283(17) 0.0331(6) Uani 0.50 1 d P . .
S7 S 0.12514(13) 0.22969(11) 0.42190(8) 0.0355(3) Uani 1 1 d . . .
N1 N 0.4442(12) 0.2179(9) 0.3828(8) 0.067(4) Uani 0.50 1 d P . .
N2 N 0.4253(11) 0.1220(7) 0.4691(6) 0.045(3) Uani 0.50 1 d P . .
O1 O 0.5000 0.2891(8) 0.2500 0.074(4) Uani 1 4 d S . .
O2 O 0.5000 0.3876(9) 0.4440(7) 0.048(4) Uani 0.50 2 d SP . .
O3 O 0.0700(13) 0.5000 0.5000 0.052(4) Uani 0.50 2 d SP . .
O4 O 0.3688(14) 0.5000 0.5000 0.053(4) Uani 0.50 2 d SP . .
O5B O 0.2104(11) 0.5714(9) 0.0950(6) 0.059(3) Uani 0.50 1 d P . .
O5A O 0.2521(12) 0.5308(9) 0.0720(6) 0.063(4) Uani 0.50 1 d P . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 '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
S3 Re1 S5 75.13(5) . . ?
S3 Re1 S5 75.13(5) . 10_556 ?
S5 Re1 S5 80.22(7) . 10_556 ?
S3 Re1 Te1 86.60(3) . 10_556 ?
S5 Re1 Te1 158.84(4) . 10_556 ?
S5 Re1 Te1 84.90(4) 10_556 10_556 ?
S3 Re1 Te1 86.60(3) . . ?
S5 Re1 Te1 84.90(4) . . ?
S5 Re1 Te1 158.84(4) 10_556 . ?
Te1 Re1 Te1 104.883(17) 10_556 . ?
S3 Re1 Te2 149.66(4) . . ?
S5 Re1 Te2 81.80(4) . . ?
S5 Re1 Te2 81.80(4) 10_556 . ?
Te1 Re1 Te2 110.961(14) 10_556 . ?
Te1 Re1 Te2 110.961(14) . . ?
S3 Re1 Re2 143.74(2) . 10_556 ?
S5 Re1 Re2 138.55(4) . 10_556 ?
S5 Re1 Re2 95.10(4) 10_556 10_556 ?
Te1 Re1 Re2 57.491(13) 10_556 10_556 ?
Te1 Re1 Re2 105.998(13) . 10_556 ?
Te2 Re1 Re2 56.839(11) . 10_556 ?
S3 Re1 Re2 143.74(2) . . ?
S5 Re1 Re2 95.10(4) . . ?
S5 Re1 Re2 138.55(4) 10_556 . ?
Te1 Re1 Re2 105.998(13) 10_556 . ?
Te1 Re1 Re2 57.491(13) . . ?
Te2 Re1 Re2 56.839(11) . . ?
Re2 Re1 Re2 61.702(14) 10_556 . ?
S3 Re1 Re1 106.82(4) . 3 ?
S5 Re1 Re1 139.81(4) . 3 ?
S5 Re1 Re1 139.81(4) 10_556 3 ?
Te1 Re1 Re1 55.700(8) 10_556 3 ?
Te1 Re1 Re1 55.700(8) . 3 ?
Te2 Re1 Re1 103.521(12) . 3 ?
Re2 Re1 Re1 58.973(6) 10_556 3 ?
Re2 Re1 Re1 58.973(6) . 3 ?
S1 Re2 S7 74.75(7) . . ?
S1 Re2 S7 74.75(7) . 12 ?
S7 Re2 S7 78.15(8) . 12 ?
S1 Re2 Te2 86.35(4) . 3 ?
S7 Re2 Te2 157.58(4) . 3 ?
S7 Re2 Te2 85.42(4) 12 3 ?
S1 Re2 Te2 86.35(4) . . ?
S7 Re2 Te2 85.42(4) . . ?
S7 Re2 Te2 157.58(4) 12 . ?
Te2 Re2 Te2 105.608(18) 3 . ?
S1 Re2 Te1 150.17(7) . . ?
S7 Re2 Te1 82.24(4) . . ?
S7 Re2 Te1 82.24(4) 12 . ?
Te2 Re2 Te1 110.751(14) 3 . ?
Te2 Re2 Te1 110.751(14) . . ?
S1 Re2 Re1 143.53(4) . 3 ?
S7 Re2 Re1 138.83(4) . 3 ?
S7 Re2 Re1 95.91(4) 12 3 ?
Te2 Re2 Re1 57.496(12) 3 3 ?
Te2 Re2 Re1 106.489(13) . 3 ?
Te1 Re2 Re1 56.610(11) . 3 ?
S1 Re2 Re1 143.53(4) . . ?
S7 Re2 Re1 95.91(4) . . ?
S7 Re2 Re1 138.83(4) 12 . ?
Te2 Re2 Re1 106.489(13) 3 . ?
Te2 Re2 Re1 57.496(12) . . ?
Te1 Re2 Re1 56.610(11) . . ?
Re1 Re2 Re1 62.055(12) 3 . ?
S1 Re2 Re2 106.54(7) . 10_556 ?
S7 Re2 Re2 140.81(4) . 10_556 ?
S7 Re2 Re2 140.81(4) 12 10_556 ?
Te2 Re2 Re2 56.072(8) 3 10_556 ?
Te2 Re2 Re2 56.072(8) . 10_556 ?
Te1 Re2 Re2 103.285(12) . 10_556 ?
Re1 Re2 Re2 59.149(7) 3 10_556 ?
Re1 Re2 Re2 59.149(7) . 10_556 ?
Re1 Te1 Re1 68.600(16) 3 . ?
Re1 Te1 Re2 65.898(13) 3 . ?
Re1 Te1 Re2 65.898(13) . . ?
Re2 Te2 Re2 67.856(17) 10_556 . ?
Re2 Te2 Re1 65.665(13) 10_556 . ?
Re2 Te2 Re1 65.665(13) . . ?
S2 S1 S2 36.95(18) 12 . ?
S2 S1 Re2 116.24(15) 12 . ?
S2 S1 Re2 116.24(15) . . ?
S2 S2 S2 90.0 12 10_556 ?
S2 S2 S1 71.52(9) 12 . ?
S2 S2 S1 132.72(12) 10_556 . ?
S2 S2 S2 51.9(2) 12 3 ?
S2 S2 S2 38.1(2) 10_556 3 ?
S1 S2 S2 109.75(17) . 3 ?
S4 S3 S4 39.42(17) . 10_556 ?
S4 S3 Re1 114.14(11) . . ?
S4 S3 Re1 114.14(11) 10_556 . ?
S4 S4 S4 90.0 10_556 12 ?
S4 S4 S3 70.29(8) 10_556 . ?
S4 S4 S3 133.89(9) 12 . ?
S4 S4 S4 48.46(16) 10_556 3 ?
S4 S4 S4 41.54(16) 12 3 ?
S3 S4 S4 107.17(16) . 3 ?
S6A S5 S6B 52.82(13) . . ?
S6A S5 Re1 111.31(11) . . ?
S6B S5 Re1 106.69(10) . . ?
S6A S6B S7 69.31(15) . . ?
S6A S6B S5 58.59(13) . . ?
S7 S6B S5 106.62(14) . . ?
S6B S6A S5 68.59(14) . . ?
S6B S6A N1 135.2(5) . . ?
S5 S6A N1 109.9(5) . . ?
S6B S6A S7 57.26(13) . . ?
S5 S6A S7 105.29(14) . . ?
N1 S6A S7 144.7(5) . . ?
S6B S7 S6A 53.43(13) . . ?
S6B S7 Re2 110.79(10) . . ?
S6A S7 Re2 107.00(11) . . ?
N1 N1 S6A 163.0(4) 12_655 . ?
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 S3 2.4839(18) . ?
Re1 S5 2.5171(14) . ?
Re1 S5 2.5171(14) 10_556 ?
Re1 Te1 2.6014(4) 10_556 ?
Re1 Te1 2.6014(4) . ?
Re1 Te2 2.6324(6) . ?
Re1 Re2 2.8440(4) 10_556 ?
Re1 Re2 2.8440(4) . ?
Re1 Re1 2.9319(5) 3 ?
Re2 S1 2.479(2) . ?
Re2 S7 2.5106(16) . ?
Re2 S7 2.5106(16) 12 ?
Re2 Te2 2.6130(4) 3 ?
Re2 Te2 2.6130(4) . ?
Re2 Te1 2.6275(6) . ?
Re2 Re1 2.8440(4) 3 ?
Re2 Re2 2.9169(6) 10_556 ?
Te1 Re1 2.6014(4) 3 ?
Te2 Re2 2.6130(4) 10_556 ?
S1 S2 2.000(5) 12 ?
S1 S2 2.000(5) . ?
S2 S2 1.268(6) 12 ?
S2 S2 1.615(8) 10_556 ?
S2 S2 2.053(7) 3 ?
S3 S4 2.034(3) . ?
S3 S4 2.034(3) 10_556 ?
S4 S4 1.372(6) 10_556 ?
S4 S4 1.549(5) 12 ?
S4 S4 2.069(6) 3 ?
S5 S6A 2.006(3) . ?
S5 S6B 2.188(3) . ?
S6B S6A 1.873(5) . ?
S6B S7 1.962(4) . ?
S6A N1 2.134(15) . ?
S6A S7 2.182(3) . ?
N1 N1 1.41(3) 12_655 ?
N2 N2 1.89(3) 12_655 ?
O3 O3 1.77(3) 9_566 ?
O5B O5A 0.959(17) . ?
