#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:43:34 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239897 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/04/4350445.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_4350445
loop_
_publ_author_name
'Hagenbach, Adelheid'
'Yegen, Eda'
'Abram, Ulrich'
_publ_section_title
;
 Technetium tetrachloride as a precursor for small technetium(IV)
 complexes.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7331
_journal_page_last               7338
_journal_paper_doi               10.1021/ic060896u
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         '[TcCl3(DMSO)3]2[TcCl6]'
_chemical_formula_sum            'C12 H36 Cl12 O6 S6 Tc3'
_chemical_formula_weight         1188.17
_chemical_name_common            '[TcCl3(DMSO)3]2[TcCl6]'
_chemical_name_systematic
;
trichlorotris(dimethylsulfoxide)technetium(IV)) hexachlorotechnetate(IV) 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                104.28(1)
_cell_angle_beta                 100.53(1)
_cell_angle_gamma                93.59(1)
_cell_formula_units_Z            1
_cell_length_a                   8.703(1)
_cell_length_b                   8.968(1)
_cell_length_c                   13.901(2)
_cell_measurement_reflns_used    7031
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.04
_cell_measurement_theta_min      3.11
_cell_volume                     1027.1(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6136
_diffrn_reflns_theta_full        24.69
_diffrn_reflns_theta_max         24.69
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    2.106
_exptl_absorpt_correction_T_max  0.8596
_exptl_absorpt_correction_T_min  0.7650
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             585
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .085
_exptl_crystal_size_min          .03
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0609
_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)+(0.0867P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                2299
_reflns_number_total             3248
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060896usi20060523_100113.cif
_cod_data_source_block           tccl3dmso
_cod_original_cell_volume        1027.7(3)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               4350445
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
Tc2 Tc 1.5000 -0.5000 0.5000 0.0334(3) Uani 1 2 d S
Cl4 Cl 1.2823(3) -0.6891(3) 0.43626(19) 0.0481(6) Uani 1 1 d .
Cl5 Cl 1.3821(3) -0.3802(3) 0.63450(19) 0.0470(6) Uani 1 1 d .
Cl6 Cl 1.3817(3) -0.3408(3) 0.40354(19) 0.0474(6) Uani 1 1 d .
Tc1 Tc 1.15244(9) 0.20185(10) 0.85746(6) 0.0384(3) Uani 1 1 d .
Cl1 Cl 0.9519(3) 0.2767(4) 0.9399(2) 0.0544(7) Uani 1 1 d .
Cl2 Cl 0.9841(3) 0.0400(4) 0.7183(2) 0.0620(8) Uani 1 1 d .
Cl3 Cl 1.2029(3) 0.0071(3) 0.9367(2) 0.0591(7) Uani 1 1 d .
S1 S 1.3574(3) 0.3437(3) 1.08140(19) 0.0465(6) Uani 1 1 d .
O1 O 1.3124(7) 0.3536(8) 0.9697(5) 0.0418(15) Uani 1 1 d .
C1 C 1.5491(16) 0.2852(18) 1.0891(9) 0.074(4) Uani 1 1 d .
H1A H 1.5423 0.1773 1.0549 0.111 Uiso 1 1 calc R
H1B H 1.5991 0.3018 1.1589 0.111 Uiso 1 1 calc R
H1C H 1.6098 0.3448 1.0576 0.111 Uiso 1 1 calc R
C2 C 1.4042(14) 0.5373(14) 1.1486(8) 0.053(3) Uani 1 1 d .
H2A H 1.3094 0.5860 1.1512 0.080 Uiso 1 1 calc R
H2B H 1.4701 0.5887 1.1154 0.080 Uiso 1 1 calc R
H2C H 1.4591 0.5440 1.2163 0.080 Uiso 1 1 calc R
S2 S 0.9848(3) 0.4222(4) 0.73525(19) 0.0468(6) Uani 1 1 d .
O2 O 1.1415(7) 0.3827(8) 0.7932(5) 0.0426(16) Uani 1 1 d .
C3 C 1.0136(14) 0.6271(14) 0.7676(9) 0.061(3) Uani 1 1 d .
H3A H 1.0044 0.6674 0.8367 0.091 Uiso 1 1 calc R
H3B H 0.9356 0.6644 0.7238 0.091 Uiso 1 1 calc R
H3C H 1.1165 0.6606 0.7598 0.091 Uiso 1 1 calc R
C4 C 1.0116(13) 0.3812(16) 0.6079(8) 0.060(3) Uani 1 1 d .
H4A H 0.9993 0.2711 0.5793 0.090 Uiso 1 1 calc R
H4B H 1.1152 0.4233 0.6068 0.090 Uiso 1 1 calc R
H4C H 0.9348 0.4269 0.5689 0.090 Uiso 1 1 calc R
S3 S 1.3679(3) -0.0008(3) 0.7260(2) 0.0511(7) Uani 1 1 d .
O3 O 1.3403(8) 0.1597(8) 0.7883(6) 0.0521(18) Uani 1 1 d .
C5 C 1.5774(14) 0.0148(16) 0.7480(12) 0.074(4) Uani 1 1 d .
H5A H 1.6182 0.0063 0.8152 0.111 Uiso 1 1 calc R
H5B H 1.6172 0.1132 0.7414 0.111 Uiso 1 1 calc R
H5C H 1.6096 -0.0667 0.6994 0.111 Uiso 1 1 calc R
C6 C 1.3240(19) 0.0141(19) 0.5994(10) 0.080(4) Uani 1 1 d .
H6A H 1.2121 0.0077 0.5771 0.121 Uiso 1 1 calc R
H6B H 1.3641 -0.0687 0.5564 0.121 Uiso 1 1 calc R
H6C H 1.3720 0.1116 0.5962 0.121 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
Cl Cl 0.1484 0.1585 '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'
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'
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
Cl4 Tc2 Cl4 180.000(1) 2_846 .
Cl4 Tc2 Cl6 88.94(9) 2_846 .
Cl4 Tc2 Cl6 91.06(9) . .
Cl4 Tc2 Cl6 91.06(9) 2_846 2_846
Cl4 Tc2 Cl6 88.94(9) . 2_846
Cl6 Tc2 Cl6 180.000(1) . 2_846
Cl4 Tc2 Cl5 90.20(9) 2_846 2_846
Cl4 Tc2 Cl5 89.80(9) . 2_846
Cl6 Tc2 Cl5 90.40(9) . 2_846
Cl6 Tc2 Cl5 89.60(9) 2_846 2_846
Cl4 Tc2 Cl5 89.80(9) 2_846 .
Cl4 Tc2 Cl5 90.20(9) . .
Cl6 Tc2 Cl5 89.60(9) . .
Cl6 Tc2 Cl5 90.40(9) 2_846 .
Cl5 Tc2 Cl5 180.00(8) 2_846 .
O2 Tc1 O1 83.4(3) . .
O2 Tc1 O3 83.5(3) . .
O1 Tc1 O3 84.5(3) . .
O2 Tc1 Cl1 92.0(2) . .
O1 Tc1 Cl1 90.9(2) . .
O3 Tc1 Cl1 173.9(2) . .
O2 Tc1 Cl2 92.0(2) . .
O1 Tc1 Cl2 173.8(2) . .
O3 Tc1 Cl2 90.9(2) . .
Cl1 Tc1 Cl2 93.39(11) . .
O2 Tc1 Cl3 171.86(19) . .
O1 Tc1 Cl3 90.4(2) . .
O3 Tc1 Cl3 90.7(2) . .
Cl1 Tc1 Cl3 93.38(11) . .
Cl2 Tc1 Cl3 93.77(12) . .
O1 S1 C2 102.6(5) . .
O1 S1 C1 102.8(5) . .
C2 S1 C1 99.6(7) . .
S1 O1 Tc1 125.2(4) . .
O2 S2 C3 102.0(5) . .
O2 S2 C4 102.8(5) . .
C3 S2 C4 99.7(6) . .
S2 O2 Tc1 123.0(4) . .
O3 S3 C6 103.2(6) . .
O3 S3 C5 101.5(5) . .
C6 S3 C5 100.4(7) . .
S3 O3 Tc1 124.6(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tc2 Cl4 2.344(2) 2_846
Tc2 Cl4 2.344(2) .
Tc2 Cl6 2.350(3) .
Tc2 Cl6 2.350(2) 2_846
Tc2 Cl5 2.357(2) 2_846
Tc2 Cl5 2.357(2) .
Tc1 O2 2.035(7) .
Tc1 O1 2.036(7) .
Tc1 O3 2.053(6) .
Tc1 Cl1 2.304(3) .
Tc1 Cl2 2.304(3) .
Tc1 Cl3 2.309(3) .
S1 O1 1.558(6) .
S1 C2 1.739(12) .
S1 C1 1.773(13) .
S2 O2 1.560(6) .
S2 C3 1.771(13) .
S2 C4 1.780(11) .
S3 O3 1.544(8) .
S3 C6 1.772(14) .
S3 C5 1.784(12) .
