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#$Date: 2016-03-25 11:25:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179789 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/85/7008535.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_7008535
loop_
_publ_author_name
'Lepareur, Nicolas'
'Mévellec, Franck'
'Noiret, Nicolas'
'Refosco, Fiorenzo'
'Tisato, Francesco'
'Porchia, Marina'
'Bandoli, Giuliano'
_publ_section_title
;
 Syntheses and reactivity of 'sulfur rich' Re(iii) and Tc(iii)
 complexes containing trithioperoxybenzoate, dithiobenzoate and
 dithiocarbamate ligands.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2866
_journal_page_last               2875
_journal_paper_doi               10.1039/b503938j
_journal_year                    2005
_chemical_formula_sum            'C21 H26 N O S8 Tc'
_chemical_formula_weight         662.91
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'heavy-atom methods'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.94(3)
_cell_angle_beta                 90.39(3)
_cell_angle_gamma                108.16(3)
_cell_formula_units_Z            2
_cell_length_a                   9.913(2)
_cell_length_b                   10.414(2)
_cell_length_c                   14.912(3)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.1
_cell_measurement_theta_min      7.7
_cell_volume                     1364.0(6)
_computing_cell_refinement       'P3/P4-PC Vers.4.27 (Nicolet, 1991)'
_computing_data_collection       'P3/P4-PC Vers.4.27 (Nicolet, 1991)'
_computing_data_reduction        'P3/P4-PC Vers.4.27 (Nicolet, 1991)'
_computing_molecular_graphics    'SHELXTL NT Vers.5.10 (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL NT Vers.5.10 (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL NT Vers.5.10 (Sheldrick, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Nicolet R3m/V four-circle diffractometer'
_diffrn_measurement_method       omega-2theta
_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  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5044
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   'psi-scan method'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0511P)²+3.6532P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                4918
_reflns_number_total             5035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b503938j.txt
_cod_data_source_block           Tc10.EtOH
_cod_original_cell_volume        1364.0(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008535
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
Tc Tc 0.14085(4) 0.68817(4) 0.21774(3) 0.04327(14) Uani 1 1 d . . .
S1 S 0.06896(14) 0.87158(13) 0.19723(10) 0.0506(3) Uani 1 1 d . . .
S2 S -0.05234(14) 0.52357(13) 0.12038(10) 0.0476(3) Uani 1 1 d . . .
S3 S -0.16586(15) 0.62245(14) 0.06239(11) 0.0556(3) Uani 1 1 d . . .
S4 S 0.21341(14) 0.50941(15) 0.24525(10) 0.0509(3) Uani 1 1 d . . .
S5 S 0.33305(15) 0.74350(15) 0.14300(11) 0.0534(3) Uani 1 1 d . . .
S6 S 0.45092(14) 0.60588(15) 0.13775(11) 0.0540(3) Uani 1 1 d . . .
S7 S 0.28744(17) 0.87544(18) 0.37106(11) 0.0658(4) Uani 1 1 d . . .
S8 S 0.00387(15) 0.68869(17) 0.35772(10) 0.0585(3) Uani 1 1 d . . .
N N 0.1538(7) 0.8824(7) 0.5273(4) 0.0882(18) Uani 1 1 d . . .
C1 C -0.0787(5) 0.8039(5) 0.1179(4) 0.0439(10) Uani 1 1 d . . .
C2 C 0.3642(5) 0.4998(5) 0.1997(4) 0.0445(10) Uani 1 1 d . . .
C3 C 0.1490(7) 0.8233(7) 0.4324(4) 0.0616(14) Uani 1 1 d . . .
C4 C 0.0289(10) 0.8301(12) 0.5764(6) 0.116(3) Uani 1 1 d . . .
H4A H -0.0579 0.7913 0.5316 0.140 Uiso 1 1 calc R . .
H4B H 0.0215 0.9117 0.6299 0.140 Uiso 1 1 calc R . .
C5 C 0.0392(14) 0.7153(15) 0.6134(9) 0.149(5) Uani 1 1 d . . .
C6 C 0.2921(10) 0.9889(11) 0.5907(7) 0.110(3) Uani 1 1 d . . .
H6A H 0.3059 0.9614 0.6451 0.132 Uiso 1 1 calc R . .
H6B H 0.3723 0.9844 0.5542 0.132 Uiso 1 1 calc R . .
C7 C 0.2892(19) 1.1285(17) 0.6235(16) 0.244(11) Uani 1 1 d . . .
C1A C -0.1389(6) 0.9009(5) 0.0918(4) 0.0479(11) Uani 1 1 d . . .
C2A C -0.0558(8) 1.0441(6) 0.1097(5) 0.0736(18) Uani 1 1 d . . .
H2AA H 0.0375 1.0794 0.1401 0.088 Uiso 1 1 calc R . .
C3A C -0.1102(9) 1.1346(7) 0.0828(6) 0.083(2) Uani 1 1 d . . .
H3AA H -0.0534 1.2303 0.0958 0.100 Uiso 1 1 calc R . .
C4A C -0.2457(9) 1.0853(8) 0.0378(5) 0.078(2) Uani 1 1 d . . .
H4AA H -0.2816 1.1472 0.0205 0.094 Uiso 1 1 calc R . .
C5A C -0.3297(8) 0.9435(9) 0.0178(6) 0.084(2) Uani 1 1 d . . .
H5AA H -0.4222 0.9093 -0.0137 0.101 Uiso 1 1 calc R . .
C6A C -0.2767(7) 0.8512(7) 0.0444(5) 0.0676(16) Uani 1 1 d . . .
H6AA H -0.3340 0.7554 0.0305 0.081 Uiso 1 1 calc R . .
C1B C 0.4313(5) 0.3987(5) 0.2121(4) 0.0464(11) Uani 1 1 d . . .
C2B C 0.3497(7) 0.2752(7) 0.2284(6) 0.0718(18) Uani 1 1 d . . .
H2BA H 0.2519 0.2557 0.2304 0.086 Uiso 1 1 calc R . .
C3B C 0.4142(8) 0.1808(7) 0.2417(6) 0.084(2) Uani 1 1 d . . .
H3BA H 0.3587 0.0990 0.2531 0.100 Uiso 1 1 calc R . .
C4B C 0.5575(8) 0.2060(8) 0.2383(6) 0.080(2) Uani 1 1 d . . .
H4BA H 0.5989 0.1404 0.2449 0.096 Uiso 1 1 calc R . .
C5B C 0.6395(7) 0.3296(8) 0.2250(6) 0.081(2) Uani 1 1 d . . .
H5BA H 0.7377 0.3495 0.2248 0.097 Uiso 1 1 calc R . .
C6B C 0.5779(6) 0.4245(7) 0.2119(5) 0.0631(15) Uani 1 1 d . . .
H6BA H 0.6352 0.5075 0.2027 0.076 Uiso 1 1 calc R . .
O O -0.3436(10) 0.5420(14) 0.4865(7) 0.178(4) Uani 1 1 d . . .
C1S C -0.413(2) 0.441(3) 0.5189(9) 0.223(10) Uani 1 1 d . . .
C2S C -0.536(3) 0.3247(19) 0.5090(11) 0.264(13) Uani 1 1 d . . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 '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
S2 Tc S5 114.02(6) . . ?
S2 Tc S1 89.45(5) . . ?
S5 Tc S1 91.51(5) . . ?
S2 Tc S4 91.96(5) . . ?
S5 Tc S4 89.69(5) . . ?
S1 Tc S4 177.60(5) . . ?
S2 Tc S8 89.22(6) . . ?
S5 Tc S8 156.53(6) . . ?
S1 Tc S8 91.99(6) . . ?
S4 Tc S8 86.09(5) . . ?
S2 Tc S7 157.85(6) . . ?
S5 Tc S7 87.97(6) . . ?
S1 Tc S7 87.21(6) . . ?
S4 Tc S7 90.76(6) . . ?
S8 Tc S7 69.04(6) . . ?
C1 S1 Tc 111.87(17) . . ?
S3 S2 Tc 110.64(7) . . ?
C1 S3 S2 104.93(18) . . ?
C2 S4 Tc 111.90(17) . . ?
S6 S5 Tc 110.11(7) . . ?
C2 S6 S5 105.19(18) . . ?
C3 S7 Tc 89.3(2) . . ?
C3 S8 Tc 89.5(2) . . ?
C3 N C4 120.5(6) . . ?
C3 N C6 121.5(7) . . ?
C4 N C6 117.4(6) . . ?
C1A C1 S1 120.7(4) . . ?
C1A C1 S3 116.5(4) . . ?
S1 C1 S3 122.8(3) . . ?
C1B C2 S4 120.8(4) . . ?
C1B C2 S6 116.2(4) . . ?
S4 C2 S6 123.0(3) . . ?
N C3 S7 123.4(5) . . ?
N C3 S8 124.4(5) . . ?
S7 C3 S8 112.2(3) . . ?
N C4 C5 113.3(9) . . ?
C7 C6 N 111.4(11) . . ?
C6A C1A C2A 118.0(5) . . ?
C6A C1A C1 121.5(5) . . ?
C2A C1A C1 120.4(5) . . ?
C3A C2A C1A 120.7(6) . . ?
C4A C3A C2A 120.7(7) . . ?
C3A C4A C5A 119.8(6) . . ?
C4A C5A C6A 120.2(7) . . ?
C5A C6A C1A 120.5(6) . . ?
C2B C1B C6B 117.5(5) . . ?
C2B C1B C2 120.4(5) . . ?
C6B C1B C2 122.0(5) . . ?
C1B C2B C3B 120.2(6) . . ?
C4B C3B C2B 121.2(6) . . ?
C3B C4B C5B 119.0(6) . . ?
C4B C5B C6B 120.6(6) . . ?
C5B C6B C1B 121.4(5) . . ?
O C1S C2S 147.5(19) . . ?
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
Tc S2 2.2208(18) . ?
Tc S5 2.2331(15) . ?
Tc S1 2.3438(13) . ?
Tc S4 2.3459(13) . ?
Tc S8 2.4973(16) . ?
Tc S7 2.508(2) . ?
S1 C1 1.674(5) . ?
S2 S3 2.0955(19) . ?
S3 C1 1.705(5) . ?
S4 C2 1.663(5) . ?
S5 S6 2.0962(19) . ?
S6 C2 1.711(5) . ?
S7 C3 1.705(6) . ?
S8 C3 1.712(6) . ?
N C3 1.331(8) . ?
N C4 1.494(10) . ?
N C6 1.524(11) . ?
C1 C1A 1.474(6) . ?
C2 C1B 1.466(7) . ?
C4 C5 1.506(16) . ?
C6 C7 1.377(17) . ?
C1A C6A 1.389(8) . ?
C1A C2A 1.390(8) . ?
C2A C3A 1.382(8) . ?
C3A C4A 1.357(11) . ?
C4A C5A 1.376(10) . ?
C5A C6A 1.389(8) . ?
C1B C2B 1.391(7) . ?
C1B C6B 1.393(7) . ?
C2B C3B 1.392(8) . ?
C3B C4B 1.367(10) . ?
C4B C5B 1.371(9) . ?
C5B C6B 1.376(8) . ?
O C1S 1.309(19) . ?
C1S C2S 1.39(2) . ?
