#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:51:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179309 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/06/4320619.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_4320619
loop_
_publ_author_name
'Yuri V. Mironov'
'Vladimir E. Fedorov'
'Ismail Ijjaali'
'James A. Ibers'
_publ_section_title
;
 [{Cu(en)2}2Re4Te4(CN)12].5H2O and [{Cu(en)2}2Re6Te8(CN)6].5H2O: Bonding
 of a Transition-Metal Complex to a Rhenium Chalcocyanide Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6320
_journal_page_last               6323
_journal_paper_doi               10.1021/ic010734s
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C14 H42 Cu2 N14 O5 Re6 Te8'
_chemical_formula_weight         2751.70
_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-97
_cell_angle_alpha                113.5990(10)
_cell_angle_beta                 103.4040(10)
_cell_angle_gamma                92.6590(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4906(3)
_cell_length_b                   10.6529(4)
_cell_length_c                   12.6252(5)
_cell_measurement_temperature    153(2)
_cell_volume                     1123.87(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13990
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    22.144
_exptl_absorpt_correction_T_max  0.4794
_exptl_absorpt_correction_T_min  0.1683
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.617
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         5372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [1.00000+0.00000exp(0.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0400P)²+0.0000sinθ/λ] 
 where P = 1.00000Fo² + 0.00000Fc² 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                4421
_reflns_number_total             5372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010734s_2.cif
_cod_data_source_block           re6
_cod_database_code               4320619
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_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 -0.15175(2) 0.60643(2) -0.51624(2) 0.01341(7) Uani 1 1 d . . .
Re2 Re 0.10835(3) 0.65261(2) -0.35696(2) 0.01335(7) Uani 1 1 d . . .
Re3 Re -0.09215(3) 0.43620(2) -0.40897(2) 0.01345(7) Uani 1 1 d . . .
Te1 Te -0.04957(5) 0.17708(4) -0.53207(4) 0.01809(10) Uani 1 1 d . . .
Te2 Te -0.35450(4) 0.38896(4) -0.56927(4) 0.01815(10) Uani 1 1 d . . .
Te3 Te 0.17076(5) 0.48153(4) -0.24881(4) 0.01913(10) Uani 1 1 d . . .
Te4 Te -0.13734(4) 0.69405(4) -0.28125(4) 0.01755(10) Uani 1 1 d . . .
C1 C -0.3152(7) 0.7321(6) -0.5223(6) 0.0197(13) Uani 1 1 d . . .
N1 N -0.3988(6) 0.8073(6) -0.5173(5) 0.0281(13) Uani 1 1 d . . .
C2 C 0.2232(7) 0.8206(6) -0.1964(6) 0.0198(13) Uani 1 1 d . . .
N2 N 0.2793(6) 0.9114(6) -0.1065(5) 0.0287(13) Uani 1 1 d . . .
C3 C -0.1913(7) 0.3650(6) -0.3073(6) 0.0195(13) Uani 1 1 d . . .
N3 N -0.2408(6) 0.3275(6) -0.2498(5) 0.0259(13) Uani 1 1 d . . .
Cu1 Cu -0.28947(9) 0.16673(8) -0.18694(7) 0.02037(17) Uani 1 1 d . . .
N11 N -0.1181(6) 0.2217(7) -0.0408(5) 0.0312(14) Uani 1 1 d . . .
H11A H -0.0811 0.3141 -0.0124 0.037 Uiso 1 1 calc R . .
H11B H -0.1479 0.2086 0.0188 0.037 Uiso 1 1 calc R . .
N12 N -0.1508(4) 0.0590(4) -0.2777(4) 0.0304(14) Uani 1 1 d . . .
H12A H -0.1711 -0.0338 -0.2960 0.036 Uiso 1 1 calc R . .
H12B H -0.1603 0.0689 -0.3480 0.036 Uiso 1 1 calc R . .
N13 N -0.4264(4) 0.2653(4) -0.0908(4) 0.0319(14) Uani 1 1 d R . .
H13A H -0.4366 0.2289 -0.0376 0.038 Uiso 1 1 d R . .
H13B H -0.3906 0.3585 -0.0483 0.038 Uiso 1 1 d R . .
N14 N -0.4723(6) 0.0638(6) -0.3207(5) 0.0258(12) Uani 1 1 d . . .
H14A H -0.4808 0.0934 -0.3807 0.031 Uiso 1 1 calc R . .
H14B H -0.4688 -0.0299 -0.3527 0.031 Uiso 1 1 calc R . .
C11 C -0.0027(9) 0.1354(9) -0.0739(8) 0.043(2) Uani 1 1 d . . .
H11C H -0.0256 0.0440 -0.0735 0.052 Uiso 1 1 calc R . .
H11D H 0.0940 0.1820 -0.0159 0.052 Uiso 1 1 calc R . .
C12 C -0.0006(8) 0.1177(8) -0.1972(7) 0.0383(19) Uani 1 1 d . . .
H12D H 0.0311 0.2084 -0.1957 0.046 Uiso 1 1 calc R . .
H12C H 0.0690 0.0544 -0.2262 0.046 Uiso 1 1 calc R . .
C13 C -0.5706(8) 0.2422(9) -0.1798(7) 0.0384(19) Uani 1 1 d . . .
H13D H -0.5676 0.3037 -0.2211 0.046 Uiso 1 1 calc R . .
H13C H -0.6495 0.2624 -0.1389 0.046 Uiso 1 1 calc R . .
C14 C -0.5983(4) 0.0924(4) -0.2690(4) 0.041(2) Uani 1 1 d . . .
H14C H -0.6101 0.0315 -0.2285 0.049 Uiso 1 1 calc R . .
H14D H -0.6895 0.0738 -0.3336 0.049 Uiso 1 1 calc R . .
O1 O 0.5834(4) 0.8160(4) -0.0695(4) 0.0490(15) Uani 1 1 d R . .
H1A H 0.6093 0.7402 -0.0705 0.074 Uiso 1 1 d R . .
H1B H 0.4861 0.8549 -0.0524 0.074 Uiso 1 1 d R . .
O2 O -0.3313(4) 0.5672(4) -0.0729(4) 0.076(2) Uani 1 1 d R . .
H2B H -0.2449 0.6011 -0.0271 0.113 Uiso 1 1 d R . .
H2A H -0.3437 0.5518 -0.1400 0.113 Uiso 1 1 d R . .
O3 O 0.0004(4) 0.5004(4) 0.0005(4) 0.165(8) Uani 1 2 d SR . .
H3A H 0.0868 0.5177 -0.0187 0.248 Uiso 0.50 1 d PR . .
H3B H 0.0867 0.4830 0.0196 0.248 Uiso 0.50 1 d PR . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
O O 0.0106 0.0060 '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'
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
C1 Re1 Re3 133.34(16) . . ?
C1 Re1 Re2 131.57(17) . . ?
Re3 Re1 Re2 60.035(9) . . ?
C1 Re1 Te3 93.16(17) . 2_564 ?
Re3 Re1 Te3 120.169(13) . 2_564 ?
Re2 Re1 Te3 120.384(13) . 2_564 ?
C1 Re1 Re2 138.45(17) . 2_564 ?
Re3 Re1 Re2 60.017(9) . 2_564 ?
Re2 Re1 Re2 89.940(10) . 2_564 ?
Te3 Re1 Re2 60.154(11) 2_564 2_564 ?
C1 Re1 Re3 136.61(16) . 2_564 ?
Re3 Re1 Re3 89.854(10) . 2_564 ?
Re2 Re1 Re3 59.959(9) . 2_564 ?
Te3 Re1 Re3 60.426(11) 2_564 2_564 ?
Re2 Re1 Re3 59.752(8) 2_564 2_564 ?
C1 Re1 Te2 91.02(16) . . ?
Re3 Re1 Te2 60.334(11) . . ?
Re2 Re1 Te2 120.369(13) . . ?
Te3 Re1 Te2 89.625(14) 2_564 . ?
Re2 Re1 Te2 60.238(11) 2_564 . ?
Re3 Re1 Te2 119.989(12) 2_564 . ?
C1 Re1 Te1 88.76(16) . 2_564 ?
Re3 Re1 Te1 120.544(13) . 2_564 ?
Re2 Re1 Te1 60.516(11) . 2_564 ?
Te3 Re1 Te1 89.256(14) 2_564 2_564 ?
Re2 Re1 Te1 119.351(12) 2_564 2_564 ?
Re3 Re1 Te1 59.606(11) 2_564 2_564 ?
Te2 Re1 Te1 178.845(15) . 2_564 ?
C1 Re1 Te4 86.20(17) . . ?
Re3 Re1 Te4 60.001(11) . . ?
Re2 Re1 Te4 60.514(11) . . ?
Te3 Re1 Te4 179.091(15) 2_564 . ?
Re2 Re1 Te4 120.017(12) 2_564 . ?
Re3 Re1 Te4 120.472(13) 2_564 . ?
Te2 Re1 Te4 89.742(14) . . ?
Te1 Re1 Te4 91.375(14) 2_564 . ?
C2 Re2 Re3 133.42(16) . . ?
C2 Re2 Re1 134.15(17) . . ?
Re3 Re2 Re1 59.901(9) . . ?
C2 Re2 Re3 136.66(16) . 2_564 ?
Re3 Re2 Re3 89.913(10) . 2_564 ?
Re1 Re2 Re3 60.196(9) . 2_564 ?
C2 Re2 Re1 135.75(17) . 2_564 ?
Re3 Re2 Re1 60.131(9) . 2_564 ?
Re1 Re2 Re1 90.060(10) . 2_564 ?
Re3 Re2 Re1 59.741(8) 2_564 2_564 ?
C2 Re2 Te3 89.29(16) . . ?
Re3 Re2 Te3 60.473(11) . . ?
Re1 Re2 Te3 120.373(13) . . ?
Re3 Re2 Te3 119.657(13) 2_564 . ?
Re1 Re2 Te3 59.918(11) 2_564 . ?
C2 Re2 Te2 91.43(16) . 2_564 ?
Re3 Re2 Te2 120.160(12) . 2_564 ?
Re1 Re2 Te2 120.368(13) . 2_564 ?
Re3 Re2 Te2 60.173(11) 2_564 2_564 ?
Re1 Re2 Te2 60.030(11) 2_564 2_564 ?
Te3 Re2 Te2 89.371(14) . 2_564 ?
C2 Re2 Te1 90.98(16) . 2_564 ?
Re3 Re2 Te1 119.954(13) . 2_564 ?
Re1 Re2 Te1 60.059(11) . 2_564 ?
Re3 Re2 Te1 59.532(11) 2_564 2_564 ?
Re1 Re2 Te1 119.272(13) 2_564 2_564 ?
Te3 Re2 Te1 178.903(15) . 2_564 ?
Te2 Re2 Te1 89.558(14) 2_564 2_564 ?
C2 Re2 Te4 88.30(16) . . ?
Re3 Re2 Te4 59.815(11) . . ?
Re1 Re2 Te4 60.090(11) . . ?
Re3 Re2 Te4 120.284(13) 2_564 . ?
Re1 Re2 Te4 119.945(12) 2_564 . ?
Te3 Re2 Te4 90.210(13) . . ?
Te2 Re2 Te4 179.505(15) 2_564 . ?
Te1 Re2 Te4 90.862(13) 2_564 . ?
C3 Re3 Re1 135.49(16) . . ?
C3 Re3 Te1 88.99(16) . . ?
Re1 Re3 Te1 120.968(13) . . ?
C3 Re3 Re2 134.63(17) . . ?
Re1 Re3 Re2 60.065(9) . . ?
Te1 Re3 Re2 120.453(12) . . ?
C3 Re3 Re2 135.28(17) . 2_564 ?
Re1 Re3 Re2 60.241(9) . 2_564 ?
Te1 Re3 Re2 60.728(11) . 2_564 ?
Re2 Re3 Re2 90.087(10) . 2_564 ?
C3 Re3 Te4 89.46(16) . . ?
Re1 Re3 Te4 60.432(11) . . ?
Te1 Re3 Te4 178.434(14) . . ?
Re2 Re3 Te4 60.670(11) . . ?
Re2 Re3 Te4 120.672(12) 2_564 . ?
C3 Re3 Re1 134.36(16) . 2_564 ?
Re1 Re3 Re1 90.146(10) . 2_564 ?
Te1 Re3 Re1 60.343(11) . 2_564 ?
Re2 Re3 Re1 60.117(8) . 2_564 ?
Re2 Re3 Re1 59.846(9) 2_564 2_564 ?
Te4 Re3 Re1 120.787(12) . 2_564 ?
C3 Re3 Te2 90.39(17) . . ?
Re1 Re3 Te2 60.230(11) . . ?
Te1 Re3 Te2 90.302(14) . . ?
Re2 Re3 Te2 120.295(12) . . ?
Re2 Re3 Te2 60.277(11) 2_564 . ?
Te4 Re3 Te2 89.928(14) . . ?
Re1 Re3 Te2 120.122(13) 2_564 . ?
C3 Re3 Te3 89.46(17) . . ?
Re1 Re3 Te3 120.121(12) . . ?
Te1 Re3 Te3 89.304(14) . . ?
Re2 Re3 Te3 60.057(11) . . ?
Re2 Re3 Te3 119.621(13) 2_564 . ?
Te4 Re3 Te3 90.462(14) . . ?
Re1 Re3 Te3 59.775(11) 2_564 . ?
Te2 Re3 Te3 179.579(14) . . ?
Re3 Te1 Re1 60.051(11) . 2_564 ?
Re3 Te1 Re2 59.740(11) . 2_564 ?
Re1 Te1 Re2 59.426(11) 2_564 2_564 ?
Re1 Te2 Re3 59.435(11) . . ?
Re1 Te2 Re2 59.732(10) . 2_564 ?
Re3 Te2 Re2 59.550(11) . 2_564 ?
Re1 Te3 Re2 59.928(11) 2_564 . ?
Re1 Te3 Re3 59.799(11) 2_564 . ?
Re2 Te3 Re3 59.470(11) . . ?
Re3 Te4 Re1 59.566(11) . . ?
Re3 Te4 Re2 59.515(10) . . ?
Re1 Te4 Re2 59.395(11) . . ?
N1 C1 Re1 175.0(6) . . ?
N2 C2 Re2 176.2(6) . . ?
N3 C3 Re3 177.9(6) . . ?
C3 N3 Cu1 151.8(5) . . ?
N14 Cu1 N11 162.8(2) . . ?
N14 Cu1 N13 85.9(2) . . ?
N11 Cu1 N13 93.7(2) . . ?
N14 Cu1 N12 94.8(2) . . ?
N11 Cu1 N12 84.5(2) . . ?
N13 Cu1 N12 176.1(2) . . ?
N14 Cu1 N3 96.5(2) . . ?
N11 Cu1 N3 100.7(2) . . ?
N13 Cu1 N3 97.01(19) . . ?
N12 Cu1 N3 86.74(19) . . ?
C11 N11 Cu1 109.0(5) . . ?
C12 N12 Cu1 106.5(4) . . ?
C13 N13 Cu1 106.2(4) . . ?
C14 N14 Cu1 107.4(4) . . ?
N11 C11 C12 106.9(6) . . ?
N12 C12 C11 108.0(6) . . ?
N13 C13 C14 107.1(5) . . ?
N14 C14 C13 108.6(4) . . ?
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 C1 2.104(6) . ?
Re1 Re3 2.6738(3) . ?
Re1 Re2 2.6782(3) . ?
Re1 Te3 2.6870(5) 2_564 ?
Re1 Re2 2.6873(3) 2_564 ?
Re1 Re3 2.6877(3) 2_564 ?
Re1 Te2 2.6954(4) . ?
Re1 Te1 2.6955(4) 2_564 ?
Re1 Te4 2.6972(5) . ?
Re2 C2 2.095(7) . ?
Re2 Re3 2.6774(3) . ?
Re2 Re3 2.6813(4) 2_564 ?
Re2 Re1 2.6873(3) 2_564 ?
Re2 Te3 2.6934(4) . ?
Re2 Te2 2.7010(4) 2_564 ?
Re2 Te1 2.7078(4) 2_564 ?
Re2 Te4 2.7086(4) . ?
Re3 C3 2.093(6) . ?
Re3 Te1 2.6756(4) . ?
Re3 Re2 2.6813(4) 2_564 ?
Re3 Te4 2.6856(4) . ?
Re3 Re1 2.6877(3) 2_564 ?
Re3 Te2 2.6982(5) . ?
Re3 Te3 2.7046(5) . ?
Te1 Re1 2.6955(4) 2_564 ?
Te1 Re2 2.7078(4) 2_564 ?
Te2 Re2 2.7010(4) 2_564 ?
Te3 Re1 2.6870(5) 2_564 ?
C1 N1 1.147(8) . ?
C2 N2 1.140(8) . ?
C3 N3 1.131(8) . ?
N3 Cu1 2.228(5) . ?
Cu1 N14 2.011(6) . ?
Cu1 N11 2.012(6) . ?
Cu1 N13 2.025(4) . ?
Cu1 N12 2.037(4) . ?
N11 C11 1.489(9) . ?
N12 C12 1.481(8) . ?
N13 C13 1.493(9) . ?
N14 C14 1.479(7) . ?
C11 C12 1.496(12) . ?
C13 C14 1.506(9) . ?
