#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:55:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179269 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/89/4318915.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_4318915
loop_
_publ_author_name
'Mehtap Emirdag-Eanes'
'James A. Ibers'
_publ_section_title
;
 Conversion of a Re(IV) Tetrahedral Cluster to a Re(III) Octahedral
 Cluster: Synthesis of [(CH3)C(NH2)2]4[Re6Se8(CN)6] by a Solvothermal
 Route
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6170
_journal_page_last               6171
_journal_paper_doi               10.1021/ic020433y
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C14 H28 N14 Re6 Se8'
_chemical_formula_weight         2141.38
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   calculated
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.7540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.3113(14)
_cell_length_b                   10.1332(7)
_cell_length_c                   19.9981(14)
_cell_measurement_temperature    153(2)
_cell_volume                     3941.3(5)
_computing_cell_refinement       'SAINT 6.22'
_computing_data_collection       'SMART 5.054'
_computing_data_reduction        'SAINT 6.22'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker 1000 CCD'
_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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23261
_diffrn_reflns_theta_full        28.86
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    25.772
_exptl_absorpt_correction_T_max  0.522
_exptl_absorpt_correction_T_min  0.098
_exptl_absorpt_correction_type   'face-indexed numerical'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3728
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.026
_refine_diff_density_max         2.720
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.379
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                3414
_reflns_number_total             4873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020433y.cif
_cod_data_source_block           '[(CH3)C(NH2)2]4[Re6Se8(CN)6]'
_cod_database_code               4318915
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.20184(2) 0.65657(4) 0.05142(2) 0.02013(11) Uani 1 1 d . . .
Re2 Re 0.332793(19) 0.68617(4) 0.05848(2) 0.02032(11) Uani 1 1 d . . .
Re3 Re 0.255239(19) 0.89565(4) 0.05872(2) 0.01944(11) Uani 1 1 d . . .
Se1 Se 0.28900(5) 0.73894(10) 0.16166(5) 0.0231(2) Uani 1 1 d . . .
Se2 Se 0.27798(5) 0.45439(9) 0.04958(5) 0.0213(2) Uani 1 1 d . . .
Se3 Se 0.12872(5) 0.86133(10) 0.04912(5) 0.0253(2) Uani 1 1 d . . .
Se4 Se 0.11864(5) 0.58053(10) -0.06429(5) 0.0235(2) Uani 1 1 d . . .
N1 N 0.1192(6) 0.4970(11) 0.1420(6) 0.060(3) Uani 1 1 d . . .
N2 N 0.4801(5) 0.5805(10) 0.1556(6) 0.050(3) Uani 1 1 d . . .
N3 N 0.2548(5) 1.1456(9) 0.1606(5) 0.038(2) Uani 1 1 d . . .
N4 N 0.0404(5) 0.3470(10) 0.2198(5) 0.045(3) Uani 1 1 d . . .
H4A H 0.0408 0.2602 0.2194 0.053 Uiso 1 1 calc R . .
H4B H 0.0669 0.3916 0.1999 0.053 Uiso 1 1 calc R . .
N5 N 0.2831(4) 0.4064(9) 0.2331(5) 0.031(2) Uani 1 1 d . . .
H5A H 0.2535 0.4607 0.2433 0.038 Uiso 1 1 calc R . .
H5B H 0.2682 0.3375 0.2063 0.038 Uiso 1 1 calc R . .
N6 N 0.3737(5) 0.5307(9) 0.2985(5) 0.033(2) Uani 1 1 d . . .
H6A H 0.3453 0.5864 0.3095 0.039 Uiso 1 1 calc R . .
H6B H 0.4184 0.5431 0.3145 0.039 Uiso 1 1 calc R . .
C1 C 0.1481(6) 0.5538(11) 0.1111(6) 0.036(3) Uani 1 1 d . . .
C2 C 0.4272(5) 0.6152(10) 0.1209(6) 0.030(2) Uani 1 1 d . . .
C3 C 0.2584(5) 1.0570(10) 0.1253(6) 0.027(2) Uani 1 1 d . . .
C4 C 0.0000 0.4103(15) 0.2500 0.035(4) Uani 1 2 d S . .
C5 C 0.0000 0.5481(18) 0.2500 0.087(9) Uani 1 2 d S . .
H5A H 0.0322 0.5803 0.2255 0.131 Uiso 0.50 1 calc PR . .
H5B H 0.0141 0.5803 0.2982 0.131 Uiso 0.50 1 calc PR . .
H5C H -0.0463 0.5803 0.2262 0.131 Uiso 0.50 1 calc PR . .
C6 C 0.3494(5) 0.4284(10) 0.2581(6) 0.027(2) Uani 1 1 d . . .
C7 C 0.3990(7) 0.3376(13) 0.2440(7) 0.059(4) Uani 1 1 d . . .
H7A H 0.3747 0.2667 0.2133 0.088 Uiso 1 1 calc R . .
H7B H 0.4272 0.2998 0.2880 0.088 Uiso 1 1 calc R . .
H7C H 0.4285 0.3851 0.2210 0.088 Uiso 1 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'
N N 0.0061 0.0033 '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'
Re Re -1.0185 7.2310 '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 Se1 90.9(3) . . ?
C1 Re1 Se3 91.0(3) . . ?
Se1 Re1 Se3 90.28(3) . . ?
C1 Re1 Se4 92.8(3) . . ?
Se1 Re1 Se4 176.30(4) . . ?
Se3 Re1 Se4 89.96(3) . . ?
C1 Re1 Se2 91.5(3) . . ?
Se1 Re1 Se2 90.15(3) . . ?
Se3 Re1 Se2 177.42(4) . . ?
Se4 Re1 Se2 89.45(3) . . ?
C1 Re1 Re2 134.7(3) . . ?
Se1 Re1 Re2 58.42(3) . . ?
Se3 Re1 Re2 118.83(3) . . ?
Se4 Re1 Re2 118.37(3) . . ?
Se2 Re1 Re2 59.39(2) . . ?
C1 Re1 Re2 135.3(3) . 7_565 ?
Se1 Re1 Re2 118.44(3) . 7_565 ?
Se3 Re1 Re2 58.59(3) . 7_565 ?
Se4 Re1 Re2 58.74(3) . 7_565 ?
Se2 Re1 Re2 119.05(3) . 7_565 ?
Re2 Re1 Re2 89.917(16) . 7_565 ?
C1 Re1 Re3 133.8(3) . . ?
Se1 Re1 Re3 58.52(2) . . ?
Se3 Re1 Re3 58.75(3) . . ?
Se4 Re1 Re3 118.67(3) . . ?
Se2 Re1 Re3 119.48(3) . . ?
Re2 Re1 Re3 60.095(14) . . ?
Re2 Re1 Re3 59.940(15) 7_565 . ?
C1 Re1 Re3 136.1(3) . 7_565 ?
Se1 Re1 Re3 118.31(3) . 7_565 ?
Se3 Re1 Re3 118.61(3) . 7_565 ?
Se4 Re1 Re3 58.48(3) . 7_565 ?
Se2 Re1 Re3 59.02(2) . 7_565 ?
Re2 Re1 Re3 59.899(15) . 7_565 ?
Re2 Re1 Re3 60.028(15) 7_565 7_565 ?
Re3 Re1 Re3 90.050(16) . 7_565 ?
C2 Re2 Se1 93.6(3) . . ?
C2 Re2 Se3 89.3(3) . 7_565 ?
Se1 Re2 Se3 177.08(4) . 7_565 ?
C2 Re2 Se4 90.9(3) . 7_565 ?
Se1 Re2 Se4 89.38(3) . 7_565 ?
Se3 Re2 Se4 90.27(3) 7_565 7_565 ?
C2 Re2 Se2 91.8(3) . . ?
Se1 Re2 Se2 90.14(3) . . ?
Se3 Re2 Se2 90.07(3) 7_565 . ?
Se4 Re2 Se2 177.30(4) 7_565 . ?
C2 Re2 Re3 133.8(3) . 7_565 ?
Se1 Re2 Re3 118.92(3) . 7_565 ?
Se3 Re2 Re3 58.86(3) 7_565 7_565 ?
Se4 Re2 Re3 119.06(3) 7_565 7_565 ?
Se2 Re2 Re3 58.99(2) . 7_565 ?
C2 Re2 Re1 136.8(3) . . ?
Se1 Re2 Re1 58.78(3) . . ?
Se3 Re2 Re1 119.01(3) 7_565 . ?
Se4 Re2 Re1 118.56(3) 7_565 . ?
Se2 Re2 Re1 59.03(2) . . ?
Re3 Re2 Re1 60.158(15) 7_565 . ?
C2 Re2 Re1 133.1(3) . 7_565 ?
Se1 Re2 Re1 118.66(3) . 7_565 ?
Se3 Re2 Re1 58.81(3) 7_565 7_565 ?
Se4 Re2 Re1 59.04(3) 7_565 7_565 ?
Se2 Re2 Re1 119.03(3) . 7_565 ?
Re3 Re2 Re1 60.038(15) 7_565 7_565 ?
Re1 Re2 Re1 90.083(16) . 7_565 ?
C2 Re2 Re3 136.0(3) . . ?
Se1 Re2 Re3 58.59(2) . . ?
Se3 Re2 Re3 118.88(3) 7_565 . ?
Se4 Re2 Re3 58.59(3) 7_565 . ?
Se2 Re2 Re3 119.00(3) . . ?
Re3 Re2 Re3 90.133(16) 7_565 . ?
Re1 Re2 Re3 59.979(14) . . ?
Re1 Re2 Re3 60.074(15) 7_565 . ?
C3 Re3 Se1 91.2(3) . . ?
C3 Re3 Se4 93.0(3) . 7_565 ?
Se1 Re3 Se4 89.46(3) . 7_565 ?
C3 Re3 Se3 90.0(3) . . ?
Se1 Re3 Se3 90.38(4) . . ?
Se4 Re3 Se3 177.02(4) 7_565 . ?
C3 Re3 Se2 91.5(3) . 7_565 ?
Se1 Re3 Se2 177.21(3) . 7_565 ?
Se4 Re3 Se2 89.84(3) 7_565 7_565 ?
Se3 Re3 Se2 90.18(3) . 7_565 ?
C3 Re3 Re2 134.2(3) . 7_565 ?
Se1 Re3 Re2 118.71(3) . 7_565 ?
Se4 Re3 Re2 119.00(3) 7_565 7_565 ?
Se3 Re3 Re2 58.61(3) . 7_565 ?
Se2 Re3 Re2 59.43(2) 7_565 7_565 ?
C3 Re3 Re1 133.4(3) . . ?
Se1 Re3 Re1 58.70(3) . . ?
Se4 Re3 Re1 118.81(3) 7_565 . ?
Se3 Re3 Re1 58.73(3) . . ?
Se2 Re3 Re1 119.45(3) 7_565 . ?
Re2 Re3 Re1 60.022(14) 7_565 . ?
C3 Re3 Re2 135.9(3) . . ?
Se1 Re3 Re2 58.42(3) . . ?
Se4 Re3 Re2 58.88(2) 7_565 . ?
Se3 Re3 Re2 118.64(3) . . ?
Se2 Re3 Re2 118.99(3) 7_565 . ?
Re2 Re3 Re2 89.867(16) 7_565 . ?
Re1 Re3 Re2 59.926(15) . . ?
C3 Re3 Re1 136.7(3) . 7_565 ?
Se1 Re3 Re1 118.31(3) . 7_565 ?
Se4 Re3 Re1 59.07(3) 7_565 7_565 ?
Se3 Re3 Re1 118.54(3) . 7_565 ?
Se2 Re3 Re1 59.10(2) 7_565 7_565 ?
Re2 Re3 Re1 59.943(15) 7_565 7_565 ?
Re1 Re3 Re1 89.950(16) . 7_565 ?
Re2 Re3 Re1 59.898(14) . 7_565 ?
Re2 Se1 Re3 62.99(3) . . ?
Re2 Se1 Re1 62.80(3) . . ?
Re3 Se1 Re1 62.78(3) . . ?
Re3 Se2 Re1 61.88(2) 7_565 . ?
Re3 Se2 Re2 61.57(2) 7_565 . ?
Re1 Se2 Re2 61.58(3) . . ?
Re2 Se3 Re1 62.60(3) 7_565 . ?
Re2 Se3 Re3 62.53(3) 7_565 . ?
Re1 Se3 Re3 62.52(3) . . ?
Re3 Se4 Re2 62.53(3) 7_565 7_565 ?
Re3 Se4 Re1 62.45(3) 7_565 . ?
Re2 Se4 Re1 62.22(3) 7_565 . ?
C4 N4 H4A 120.0 . . ?
C4 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C6 N5 H5A 120.0 . . ?
C6 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C6 N6 H6A 120.0 . . ?
C6 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
N1 C1 Re1 178.6(11) . . ?
N2 C2 Re2 177.7(10) . . ?
N3 C3 Re3 174.9(10) . . ?
N4 C4 N4 121.7(15) . 2 ?
N4 C4 C5 119.1(7) . . ?
N4 C4 C5 119.1(7) 2 . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N5 C6 N6 121.8(10) . . ?
N5 C6 C7 120.8(11) . . ?
N6 C6 C7 117.3(10) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
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 2.111(12) . ?
Re1 Se1 2.5379(11) . ?
Re1 Se3 2.5444(11) . ?
Re1 Se4 2.5592(11) . ?
Re1 Se2 2.5735(10) . ?
Re1 Re2 2.6396(6) . ?
Re1 Re2 2.6406(6) 7_565 ?
Re1 Re3 2.6410(5) . ?
Re1 Re3 2.6453(6) 7_565 ?
Re2 C2 2.091(10) . ?
Re2 Se1 2.5284(11) . ?
Re2 Se3 2.5383(11) 7_565 ?
Re2 Se4 2.5514(11) 7_565 ?
Re2 Se2 2.5832(10) . ?
Re2 Re3 2.6384(6) 7_565 ?
Re2 Re1 2.6406(6) 7_565 ?
Re2 Re3 2.6441(5) . ?
Re3 C3 2.097(10) . ?
Re3 Se1 2.5330(10) . ?
Re3 Se4 2.5434(11) 7_565 ?
Re3 Se3 2.5451(11) . ?
Re3 Se2 2.5715(10) 7_565 ?
Re3 Re2 2.6384(6) 7_565 ?
Re3 Re1 2.6453(6) 7_565 ?
Se2 Re3 2.5715(10) 7_565 ?
Se3 Re2 2.5383(11) 7_565 ?
Se4 Re3 2.5434(11) 7_565 ?
Se4 Re2 2.5514(11) 7_565 ?
N1 C1 1.124(14) . ?
N2 C2 1.153(13) . ?
N3 C3 1.157(13) . ?
N4 C4 1.317(12) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N5 C6 1.314(12) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N6 C6 1.320(13) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
C4 N4 1.317(12) 2 ?
C4 C5 1.40(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.451(15) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
