#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:30:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179331 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/28/4322898.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_4322898
loop_
_publ_author_name
'Roger Schibli'
'Roger Alberto'
'Ulrich Abram'
'Sonja Abram'
'André Egli'
'P. August Schubiger'
'Thomas A. Kaden'
_publ_section_title
;
 Structural and 99Tc NMR Investigations of Complexes with fac-[Tc(CO)3]+
 Moieties and Macrocyclic Thioethers of Various Ring Sizes: Synthesis and
 X-ray Structure of the Complexes fac-[Tc(9-ane-S3)(CO)3]Br,
 fac-[Tc2(tosylate)2(18-ane-S6)(CO)6], and
 fac-[Tc2(20-ane-S6-OH)(CO)6][tosylate]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3509
_journal_page_last               3516
_journal_paper_doi               10.1021/ic980112f
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety
'[Tc2(CO)6(20ane-S6-OH)](O3S(C6H4)CH3)2 x MeOH'
_chemical_formula_sum            'C35 H46 O14 S8 Tc2'
_chemical_formula_weight         1143.20
_chemical_name_systematic
; 
[Tc2(20ane-S6-OH)(CO)6](tosylate)2 x MeOH 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 149.56(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.737(4)
_cell_length_b                   14.009(1)
_cell_length_c                   26.479(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      13.74
_cell_measurement_theta_min      7.71
_cell_volume                     4837(3)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4
_computing_data_reduction        'PLATON,HELENA (Spek, 1995)'
_computing_molecular_graphics
'SCHAKAL (Keller, 1995), ZORTEP (Zsolnai,1997)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18103
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        5.0
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.685
_refine_diff_density_min         -.916
_refine_diff_density_rms         .165
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(6)
_refine_ls_extinction_coef       0.0051(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²l³/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.056
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         16885
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.145
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_obs          0.0725
_refine_ls_shift/esd_max         -0.053
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s²(Fo²)+( 0.1362P)²+1.1401P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2239
_refine_ls_wR_factor_obs         0.1792
_reflns_number_observed          12860
_reflns_number_total             17032
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980112f_3.cif
_cod_data_source_block           '[Tc2(20-ane-S6-OH)(CO)6](tosylate)2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1362P)^2^+1.1401P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.1362P)^2^+1.1401P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4836(1)
_cod_database_code               4322898
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Tc1 Tc 0.40511(6) 0.70498(6) 0.52622(5) 0.0211(2) Uani 1 d . .
Tc2 Tc 0.29867(7) 0.79885(7) 0.19169(6) 0.0297(2) Uani 1 d . .
S1 S 0.3043(3) 0.6160(3) 0.3777(3) 0.0485(9) Uani 1 d . .
S5 S 0.2564(3) 0.6735(3) 0.2175(3) 0.0567(10) Uani 1 d . .
S8 S 0.2810(4) 0.6703(4) 0.1150(4) 0.0729(13) Uani 1 d . .
S11 S 0.4815(4) 0.7498(4) 0.3474(4) 0.0665(12) Uani 1 d . .
S15 S 0.5680(3) 0.6684(3) 0.6186(3) 0.0536(10) Uani 1 d . .
S18 S 0.4269(3) 0.5455(3) 0.5819(3) 0.0555(10) Uani 1 d . .
C2 C 0.1769(12) 0.6639(13) 0.2729(13) 0.064(5) Uani 1 d . .
H2A H 0.1429(12) 0.6408(13) 0.2751(13) 0.077 Uiso 1 calc R .
H2B H 0.1812(12) 0.7336(13) 0.2789(13) 0.077 Uiso 1 calc R .
C3 C 0.1104(13) 0.6375(12) 0.1714(13) 0.055(4) Uani 1 d . .
H3 H 0.0382(13) 0.6485(12) 0.1209(13) 0.067 Uiso 1 calc R .
C4 C 0.1284(13) 0.6946(17) 0.1387(14) 0.073(6) Uani 1 d . .
H4A H 0.1214(13) 0.7627(17) 0.1405(14) 0.088 Uiso 1 calc R .
H4B H 0.0755(13) 0.6781(17) 0.0695(14) 0.088 Uiso 1 calc R .
C6 C 0.2349(18) 0.5647(13) 0.1646(19) 0.085(6) Uani 1 d . .
H6A H 0.2980(18) 0.5266(13) 0.2173(19) 0.102 Uiso 1 calc R .
H6B H 0.1814(18) 0.5272(13) 0.1365(19) 0.102 Uiso 1 calc R .
C7 C 0.2003(15) 0.5871(15) 0.0778(15) 0.075(5) Uani 1 d . .
H7A H 0.1300(15) 0.6120(15) 0.0191(15) 0.090 Uiso 1 calc R .
H7B H 0.2003(15) 0.5274(15) 0.0586(15) 0.090 Uiso 1 calc R .
C9 C 0.4043(15) 0.6075(13) 0.2176(15) 0.063(5) Uani 1 d . .
H9A H 0.4045(15) 0.5580(13) 0.2439(15) 0.075 Uiso 1 calc R .
H9B H 0.4139(15) 0.5764(13) 0.1928(15) 0.075 Uiso 1 calc R .
C10 C 0.4968(19) 0.6805(18) 0.3051(19) 0.095(8) Uani 1 d . .
H10A H 0.5029(19) 0.7234(18) 0.2811(19) 0.114 Uiso 1 calc R .
H10B H 0.5609(19) 0.6443(18) 0.3614(19) 0.114 Uiso 1 calc R .
C12 C 0.5067(15) 0.6586(14) 0.4152(15) 0.067(5) Uani 1 d . .
H12A H 0.4486(15) 0.6144(14) 0.3677(15) 0.080 Uiso 1 calc R .
H12B H 0.5676(15) 0.6222(14) 0.4561(15) 0.080 Uiso 1 calc R .
C13 C 0.5244(13) 0.7011(12) 0.4831(11) 0.051(4) Uani 1 d . .
H13A H 0.5789(13) 0.7492(12) 0.5274(11) 0.062 Uiso 1 calc R .
H13B H 0.4615(13) 0.7320(12) 0.4424(11) 0.062 Uiso 1 calc R .
C14 C 0.5536(14) 0.6236(12) 0.5422(13) 0.055(4) Uani 1 d . .
H14A H 0.6184(14) 0.5953(12) 0.5853(13) 0.066 Uiso 1 calc R .
H14B H 0.5010(14) 0.5737(12) 0.4974(13) 0.066 Uiso 1 calc R .
C16 C 0.6093(12) 0.5653(13) 0.6863(11) 0.056(4) Uani 1 d . .
H16A H 0.6648(12) 0.5349(13) 0.7138(11) 0.068 Uiso 1 calc R .
H16B H 0.6372(12) 0.5849(13) 0.7425(11) 0.068 Uiso 1 calc R .
C17 C 0.5256(12) 0.4934(12) 0.6249(11) 0.052(4) Uani 1 d . .
H17A H 0.5540(12) 0.4366(12) 0.6651(11) 0.062 Uiso 1 calc R .
H17B H 0.4960(12) 0.4742(12) 0.5676(11) 0.062 Uiso 1 calc R .
C19 C 0.3094(13) 0.4875(12) 0.4641(13) 0.064(5) Uani 1 d . .
H19A H 0.3139(13) 0.4196(12) 0.4764(13) 0.077 Uiso 1 calc R .
H19B H 0.2524(13) 0.5147(12) 0.4357(13) 0.077 Uiso 1 calc R .
C20 C 0.2849(13) 0.4969(11) 0.3863(12) 0.052(4) Uani 1 d . .
H20A H 0.2134(13) 0.4783(11) 0.3207(12) 0.063 Uiso 1 calc R .
H20B H 0.3284(13) 0.4523(11) 0.4040(12) 0.063 Uiso 1 calc R .
O1 O 0.1183(12) 0.5406(12) 0.1644(12) 0.104(5) Uani 1 d . .
H1 H 0.1089(12) 0.5067(12) 0.1818(12) 0.156 Uiso 1 calc R .
C101 C 0.2858(13) 0.7281(12) 0.4653(12) 0.054(4) Uani 1 d . .
C102 C 0.3833(14) 0.8276(14) 0.4728(14) 0.064(5) Uani 1 d . .
C103 C 0.4868(15) 0.7716(14) 0.6445(15) 0.066(5) Uani 1 d . .
C104 C 0.3212(15) 0.8918(14) 0.2610(13) 0.063(4) Uani 1 d . .
C105 C 0.1591(20) 0.8320(15) 0.0662(17) 0.079(6) Uani 1 d . .
C106 C 0.3292(15) 0.8912(16) 0.1689(15) 0.074(6) Uani 1 d . .
O101 O 0.2184(11) 0.7463(10) 0.4340(11) 0.078(4) Uani 1 d . .
O102 O 0.3671(13) 0.8951(10) 0.4368(12) 0.089(4) Uani 1 d . .
O103 O 0.5320(13) 0.8119(11) 0.7126(11) 0.093(5) Uani 1 d . .
O104 O 0.3324(15) 0.9490(12) 0.3025(13) 0.107(5) Uani 1 d . .
O105 O 0.0690(11) 0.8588(12) -0.0139(11) 0.089(4) Uani 1 d . .
O106 O 0.3458(13) 0.9496(12) 0.1517(12) 0.097(5) Uani 1 d . .
S41 S 0.5152(3) 0.7648(3) 0.1790(3) 0.0583(10) Uani 1 d . .
O41 O 0.6045(9) 0.7086(11) 0.2616(9) 0.083(4) Uani 1 d . .
O42 O 0.4323(11) 0.7097(10) 0.0931(10) 0.097(5) Uani 1 d . .
O43 O 0.4892(13) 0.8208(9) 0.2011(13) 0.091(5) Uani 1 d . .
C42 C 0.5630(11) 0.9378(12) 0.1771(12) 0.055(4) Uani 1 d . .
H42 H 0.5575(11) 0.9615(12) 0.2056(12) 0.066 Uiso 1 calc R .
C41 C 0.5451(11) 0.8427(11) 0.1539(11) 0.052(4) Uani 1 d . .
C43 C 0.5890(15) 1.0005(15) 0.1603(14) 0.077(6) Uani 1 d . .
H43 H 0.5978(15) 1.0659(15) 0.1746(14) 0.092 Uiso 1 calc R .
C44 C 0.6015(15) 0.9664(16) 0.1229(14) 0.072(5) Uani 1 d . .
C45 C 0.5850(15) 0.8682(15) 0.1000(13) 0.074(6) Uani 1 d . .
H45 H 0.5912(15) 0.8434(15) 0.0724(13) 0.089 Uiso 1 calc R .
C46 C 0.5586(16) 0.8063(18) 0.1195(14) 0.077(6) Uani 1 d . .
H46 H 0.5509(16) 0.7403(18) 0.1078(14) 0.092 Uiso 1 calc R .
C47 C 0.6203(3) 1.0288(3) 0.0909(3) 0.122(11) Uani 1 d . .
H47A H 0.6267(3) 0.9879(3) 0.0669(3) 0.183 Uiso 1 calc R .
H47B H 0.6829(3) 1.0653(3) 0.1477(3) 0.183 Uiso 1 calc R .
H47C H 0.5631(3) 1.0721(3) 0.0382(3) 0.183 Uiso 1 calc R .
S51 S 0.8877(3) 0.4124(3) 0.3395(3) 0.0703(13) Uani 1 d R .
O51 O 0.7984(3) 0.4748(3) 0.2593(3) 0.084(4) Uani 1 d R .
O52 O 0.9082(3) 0.3524(3) 0.3128(3) 0.132(7) Uani 1 d R .
O53 O 0.9794(3) 0.4607(3) 0.4353(3) 0.120(7) Uani 1 d R .
C51 C 0.8596(3) 0.3300(3) 0.3643(3) 0.055(4) Uani 1 d R .
C52 C 0.8370(3) 0.2362(3) 0.3366(3) 0.093(7) Uani 1 d R .
H52 H 0.8336(3) 0.2117(3) 0.3007(3) 0.111 Uiso 1 calc R .
C53 C 0.8193(19) 0.1788(17) 0.3630(19) 0.084(6) Uani 1 d . .
H53 H 0.8128(19) 0.1127(17) 0.3523(19) 0.101 Uiso 1 calc R .
C54 C 0.8106(16) 0.2135(19) 0.4046(18) 0.106(10) Uani 1 d . .
C55 C 0.8252(16) 0.3054(20) 0.4266(16) 0.085(7) Uani 1 d . .
H55 H 0.8157(16) 0.3285(20) 0.4516(16) 0.102 Uiso 1 calc R .
C56 C 0.8557(12) 0.3706(16) 0.4122(12) 0.074(6) Uani 1 d . .
H56 H 0.8718(12) 0.4349(16) 0.4323(12) 0.088 Uiso 1 calc R .
C57 C 0.7872(19) 0.1415(17) 0.4274(18) 0.110(9) Uani 1 d . .
H57A H 0.7790(19) 0.0783(17) 0.4062(18) 0.165 Uiso 1 calc R .
H57B H 0.7244(19) 0.1600(17) 0.3919(18) 0.165 Uiso 1 calc R .
H57C H 0.8434(19) 0.1410(17) 0.4985(18) 0.165 Uiso 1 calc R .
Tc4 Tc -0.00036(6) 0.11340(6) -0.00050(6) 0.0224(2) Uani 1 d . .
Tc3 Tc 0.11583(6) 0.02578(7) 0.34198(6) 0.0261(2) Uani 1 d . .
S25 S 0.1044(3) 0.2094(3) 0.1459(3) 0.0520(10) Uani 1 d . .
S21 S 0.1496(3) 0.1411(3) 0.3021(3) 0.0509(9) Uani 1 d . .
S38 S 0.1328(3) 0.1658(3) 0.4113(3) 0.0567(10) Uani 1 d . .
S35 S -0.0694(3) 0.0642(3) 0.1873(3) 0.0565(10) Uani 1 d . .
S31 S -0.1609(3) 0.1536(4) -0.0893(3) 0.0585(11) Uani 1 d . .
S28 S -0.0266(3) 0.2677(3) -0.0646(3) 0.0576(10) Uani 1 d . .
C24 C 0.2294(12) 0.1542(11) 0.2523(11) 0.048(4) Uani 1 d . .
H24A H 0.2196(12) 0.0848(11) 0.2439(11) 0.058 Uiso 1 calc R .
H24B H 0.2652(12) 0.1709(11) 0.2509(11) 0.058 Uiso 1 calc R .
C23 C 0.2985(13) 0.1786(13) 0.3535(12) 0.056(4) Uani 1 d . .
H23 H 0.3694(13) 0.1622(13) 0.4029(12) 0.067 Uiso 1 calc R .
C22 C 0.2752(13) 0.1248(11) 0.3830(12) 0.053(4) Uani 1 d . .
H22A H 0.3245(13) 0.1452(11) 0.4501(12) 0.064 Uiso 1 calc R .
H22B H 0.2860(13) 0.0565(11) 0.3862(12) 0.064 Uiso 1 calc R .
C40 C 0.1617(16) 0.2517(12) 0.3437(16) 0.072(5) Uani 1 d . .
H40A H 0.2111(16) 0.2911(12) 0.3667(16) 0.086 Uiso 1 calc R .
H40B H 0.0953(16) 0.2845(12) 0.2869(16) 0.086 Uiso 1 calc R .
C39 C 0.1952(15) 0.2459(14) 0.4258(14) 0.070(5) Uani 1 d . .
H39A H 0.1876(15) 0.3094(14) 0.4345(14) 0.084 Uiso 1 calc R .
H39B H 0.2684(15) 0.2302(14) 0.4877(14) 0.084 Uiso 1 calc R .
C37 C -0.0004(15) 0.2175(17) 0.3018(15) 0.079(6) Uani 1 d . .
H37A H -0.0093(15) 0.2551(17) 0.3252(15) 0.095 Uiso 1 calc R .
H37B H -0.0114(15) 0.2597(17) 0.2636(15) 0.095 Uiso 1 calc R .
C36 C -0.0761(14) 0.1372(14) 0.2373(15) 0.070(5) Uani 1 d . .
H36A H -0.1454(14) 0.1638(14) 0.1819(15) 0.084 Uiso 1 calc R .
H36B H -0.0648(14) 0.0967(14) 0.2765(15) 0.084 Uiso 1 calc R .
C34 C -0.1100(14) 0.1502(13) 0.1051(13) 0.064(4) Uani 1 d . .
H34A H -0.1776(14) 0.1751(13) 0.0577(13) 0.077 Uiso 1 calc R .
H34B H -0.0619(14) 0.2040(13) 0.1455(13) 0.077 Uiso 1 calc R .
C33 C -0.1158(16) 0.1105(13) 0.0478(16) 0.071(5) Uani 1 d . .
H33A H -0.1677(16) 0.0600(13) 0.0028(16) 0.085 Uiso 1 calc R .
H33B H -0.0495(16) 0.0833(13) 0.0937(16) 0.085 Uiso 1 calc R .
C32 C -0.1445(13) 0.1919(14) -0.0116(13) 0.063(5) Uani 1 d . .
H32A H -0.0907(13) 0.2407(14) 0.0347(13) 0.076 Uiso 1 calc R .
H32B H -0.2084(13) 0.2213(14) -0.0533(13) 0.076 Uiso 1 calc R .
C30 C -0.2010(18) 0.2696(24) -0.1491(21) 0.142(14) Uani 1 d . .
H30A H -0.2753(18) 0.2675(24) -0.2169(21) 0.171 Uiso 1 calc R .
H30B H -0.1880(18) 0.3187(24) -0.1126(21) 0.171 Uiso 1 calc R .
C29 C -0.1511(35) 0.3003(27) -0.1553(46) 0.301(39) Uani 1 d . .
H29A H -0.1539(35) 0.3702(27) -0.1586(46) 0.361 Uiso 1 calc R .
H29B H -0.1941(35) 0.2771(27) -0.2191(46) 0.361 Uiso 1 calc R .
C27 C 0.0542(26) 0.3541(24) 0.0357(19) 0.148(14) Uani 1 d . .
H27A H 0.0904(26) 0.3924(24) 0.0406(19) 0.177 Uiso 1 calc R .
H27B H 0.0102(26) 0.3974(24) 0.0181(19) 0.177 Uiso 1 calc R .
C26 C 0.1223(17) 0.3166(15) 0.1235(17) 0.079(6) Uani 1 d . .
H26A H 0.1401(17) 0.3671(15) 0.1625(17) 0.095 Uiso 1 calc R .
H26B H 0.1838(17) 0.3054(15) 0.1546(17) 0.095 Uiso 1 calc R .
O21 O 0.2944(11) 0.2807(10) 0.3580(11) 0.079(4) Uani 1 d . .
H21 H 0.3323(11) 0.2954(10) 0.4137(11) 0.118 Uiso 1 calc R .
O205 O 0.1914(11) 0.0689(12) 0.0961(10) 0.083(4) Uani 1 d . .
O204 O 0.0417(11) -0.0691(11) 0.0934(10) 0.082(4) Uani 1 d . .
O206 O -0.1285(11) 0.0046(12) -0.1868(10) 0.087(4) Uani 1 d . .
O203 O 0.0906(13) -0.1087(11) 0.4111(12) 0.099(5) Uani 1 d . .
O201 O 0.3426(11) -0.0321(10) 0.5389(11) 0.078(4) Uani 1 d . .
O202 O 0.0720(13) -0.1366(10) 0.2297(12) 0.094(5) Uani 1 d . .
C205 C 0.1219(13) 0.0882(14) 0.0616(13) 0.063(5) Uani 1 d . .
C204 C 0.0248(14) 0.0018(14) 0.0569(13) 0.062(4) Uani 1 d . .
C206 C -0.0815(14) 0.0434(16) -0.1167(13) 0.074(6) Uani 1 d . .
C203 C 0.0983(16) -0.0609(14) 0.3832(14) 0.069(5) Uani 1 d . .
C201 C 0.2589(14) -0.0053(14) 0.4670(13) 0.061(4) Uani 1 d . .
C202 C 0.0920(14) -0.0772(14) 0.2761(14) 0.073(5) Uani 1 d . .
S61 S 0.9541(4) 0.4541(3) 0.1246(4) 0.0667(12) Uani 1 d . .
O61 O 0.9659(11) 0.4386(10) 0.0811(12) 0.086(4) Uani 1 d . .
O62 O 1.0299(11) 0.5191(11) 0.2067(11) 0.086(4) Uani 1 d . .
O63 O 0.9530(12) 0.3648(11) 0.1513(13) 0.108(6) Uani 1 d . .
C61 C 0.8322(15) 0.5066(14) 0.0324(14) 0.070(5) Uani 1 d . .
C62 C 0.8260(20) 0.5894(15) 0.0565(19) 0.086(6) Uani 1 d . .
H62 H 0.8837(20) 0.6191(15) 0.1192(19) 0.103 Uiso 1 calc R .
C63 C 0.7262(18) 0.6241(16) -0.0208(17) 0.082(6) Uani 1 d . .
H63 H 0.7166(18) 0.6760(16) -0.0068(17) 0.098 Uiso 1 calc R .
C64 C 0.6436(16) 0.5886(14) -0.1133(16) 0.069(5) Uani 1 d . .
C65 C 0.6504(14) 0.5041(15) -0.1375(14) 0.068(5) Uani 1 d . .
H65 H 0.5922(14) 0.4763(15) -0.2012(14) 0.082 Uiso 1 calc R .
C66 C 0.7474(14) 0.4652(13) -0.0620(14) 0.067(5) Uani 1 d . .
H66 H 0.7561(14) 0.4103(13) -0.0746(14) 0.080 Uiso 1 calc R .
C67 C 0.5316(23) 0.6257(18) -0.1949(21) 0.113(9) Uani 1 d . .
H67A H 0.4824(23) 0.5914(18) -0.2568(21) 0.170 Uiso 1 calc R .
H67B H 0.5273(23) 0.6934(18) -0.2059(21) 0.170 Uiso 1 calc R .
H67C H 0.5166(23) 0.6150(18) -0.1721(21) 0.170 Uiso 1 calc R .
S71 S 0.4512(4) 0.3617(4) 0.3891(4) 0.0674(12) Uani 1 d . .
O71 O 0.3787(12) 0.2875(12) 0.3125(12) 0.094(5) Uani 1 d . .
O72 O 0.4504(12) 0.4428(11) 0.3591(13) 0.097(5) Uani 1 d . .
O73 O 0.4440(13) 0.3850(13) 0.4365(14) 0.105(5) Uani 1 d . .
C71 C 0.5720(15) 0.3126(13) 0.4830(16) 0.068(5) Uani 1 d . .
C72 C 0.5901(18) 0.2271(16) 0.4752(17) 0.078(6) Uani 1 d . .
H72 H 0.5340(18) 0.1907(16) 0.4169(17) 0.093 Uiso 1 calc R .
C73 C 0.6878(25) 0.1923(18) 0.5500(23) 0.106(9) Uani 1 d . .
H73 H 0.6957(25) 0.1323(18) 0.5412(23) 0.127 Uiso 1 calc R .
C74 C 0.7738(19) 0.2410(21) 0.6363(18) 0.087(7) Uani 1 d . .
C75 C 0.7582(21) 0.3199(20) 0.6475(18) 0.103(8) Uani 1 d . .
H75 H 0.8157(21) 0.3529(20) 0.7081(18) 0.123 Uiso 1 calc R .
C76 C 0.6575(21) 0.3607(20) 0.5722(19) 0.115(10) Uani 1 d . .
H76 H 0.6506(21) 0.4187(20) 0.5840(19) 0.138 Uiso 1 calc R .
C77 C 0.8701(23) 0.2024(24) 0.7084(24) 0.144(13) Uani 1 d . .
H77A H 0.8632(23) 0.1433(24) 0.6839(24) 0.217 Uiso 1 calc R .
H77B H 0.9033(23) 0.1896(24) 0.7684(24) 0.217 Uiso 1 calc R .
H77C H 0.9111(23) 0.2472(24) 0.7235(24) 0.217 Uiso 1 calc R .
O200 O 0.7573(13) 0.3154(13) 0.1191(14) 0.042(4) Uani 0.50 d PD .
H200 H 0.7241(13) 0.2684(13) 0.0813(14) 0.063 Uiso 0.50 calc PR .
C200 C 0.7698(21) 0.3752(32) 0.0922(25) 0.095(17) Uani 0.50 d PD .
H20C H 0.7259(21) 0.4303(32) 0.0605(25) 0.143 Uiso 0.50 calc PR .
H20D H 0.7518(21) 0.3441(32) 0.0456(25) 0.143 Uiso 0.50 calc PR .
H20E H 0.8408(21) 0.3955(32) 0.1505(25) 0.143 Uiso 0.50 calc PR .
O300 O 0.0973(20) 0.4850(27) 0.3635(17) 0.105(12) Uani 0.50 d PD .
H300 H 0.0676(20) 0.4683(27) 0.3124(17) 0.157 Uiso 0.50 calc PR .
C300 C 0.0387(29) 0.5403(35) 0.3399(26) 0.089(15) Uani 0.50 d PD .
H30C H 0.0142(29) 0.5070(35) 0.3491(26) 0.134 Uiso 0.50 calc PR .
H30D H -0.0192(29) 0.5591(35) 0.2706(26) 0.134 Uiso 0.50 calc PR .
H30E H 0.0768(29) 0.5966(35) 0.3819(26) 0.134 Uiso 0.50 calc PR .
O400 O 0.2822(27) 0.3572(24) 0.1408(27) 0.114(11) Uani 0.50 d PD .
H400 H 0.3427(27) 0.3659(24) 0.2000(27) 0.170 Uiso 0.50 calc PR .
C400 C 0.2764(45) 0.2834(32) 0.1080(45) 0.114(20) Uani 0.50 d PD .
H40C H 0.2060(45) 0.2745(32) 0.0382(45) 0.171 Uiso 0.50 calc PR .
H40D H 0.2987(45) 0.2279(32) 0.1457(45) 0.171 Uiso 0.50 calc PR .
H40E H 0.3200(45) 0.2918(32) 0.1152(45) 0.171 Uiso 0.50 calc PR .
O500 O 0.6468(18) 0.8975(23) 0.3895(19) 0.090(10) Uani 0.50 d PD .
H500 H 0.7042(18) 0.9057(23) 0.4247(19) 0.136 Uiso 0.50 calc PR .
C500 C 0.6180(35) 0.9748(35) 0.3875(36) 0.147(29) Uani 0.50 d PD .
H50A H 0.5634(35) 0.9603(35) 0.3654(36) 0.220 Uiso 0.50 calc PR .
H50B H 0.5933(35) 1.0199(35) 0.3419(36) 0.220 Uiso 0.50 calc PR .
H50C H 0.6756(35) 1.0023(35) 0.4539(36) 0.220 Uiso 0.50 calc PR .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 .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
C101 Tc1 C103 89.9(8) . . ?
C101 Tc1 C102 89.4(7) . . ?
C103 Tc1 C102 88.9(8) . . ?
C101 Tc1 S18 91.8(5) . . ?
C103 Tc1 S18 95.8(6) . . ?
C102 Tc1 S18 175.2(5) . . ?
C101 Tc1 S15 174.9(5) . . ?
C103 Tc1 S15 87.1(6) . . ?
C102 Tc1 S15 94.7(5) . . ?
S18 Tc1 S15 84.41(14) . . ?
C101 Tc1 S1 91.4(5) . . ?
C103 Tc1 S1 178.3(6) . . ?
C102 Tc1 S1 92.2(5) . . ?
S18 Tc1 S1 83.10(15) . . ?
S15 Tc1 S1 91.56(14) . . ?
C106 Tc2 C104 88.5(9) . . ?
C106 Tc2 C105 87.3(8) . . ?
C104 Tc2 C105 93.7(8) . . ?
C106 Tc2 S8 94.1(7) . . ?
C104 Tc2 S8 175.1(6) . . ?
C105 Tc2 S8 90.6(6) . . ?
C106 Tc2 S5 178.0(7) . . ?
C104 Tc2 S5 93.5(5) . . ?
C105 Tc2 S5 92.2(6) . . ?
S8 Tc2 S5 84.0(2) . . ?
C106 Tc2 S11 90.3(6) . . ?
C104 Tc2 S11 91.3(6) . . ?
C105 Tc2 S11 174.4(5) . . ?
S8 Tc2 S11 84.5(2) . . ?
S5 Tc2 S11 89.99(15) . . ?
C2 S1 C20 101.8(8) . . ?
C2 S1 Tc1 106.4(7) . . ?
C20 S1 Tc1 106.7(5) . . ?
C6 S5 C4 101.7(11) . . ?
C6 S5 Tc2 107.6(6) . . ?
C4 S5 Tc2 110.9(7) . . ?
C7 S8 C9 102.2(9) . . ?
C7 S8 Tc2 103.6(6) . . ?
C9 S8 Tc2 106.1(7) . . ?
C10 S11 C12 99.0(9) . . ?
C10 S11 Tc2 103.8(8) . . ?
C12 S11 Tc2 112.9(6) . . ?
C16 S15 C14 102.3(8) . . ?
C16 S15 Tc1 101.2(6) . . ?
C14 S15 Tc1 115.0(6) . . ?
C19 S18 C17 104.9(8) . . ?
C19 S18 Tc1 101.3(6) . . ?
C17 S18 Tc1 102.4(5) . . ?
C3 C2 S1 114.1(13) . . ?
O1 C3 C4 106.5(16) . . ?
O1 C3 C2 113.1(16) . . ?
C4 C3 C2 116.5(15) . . ?
C3 C4 S5 113.2(13) . . ?
C7 C6 S5 111.2(13) . . ?
C6 C7 S8 113.1(13) . . ?
C10 C9 S8 110.6(12) . . ?
C9 C10 S11 113.7(14) . . ?
C13 C12 S11 112.2(13) . . ?
C14 C13 C12 108.8(14) . . ?
C13 C14 S15 110.8(11) . . ?
C17 C16 S15 113.6(11) . . ?
C16 C17 S18 109.5(12) . . ?
C20 C19 S18 114.3(11) . . ?
C19 C20 S1 113.9(10) . . ?
O101 C101 Tc1 175.3(16) . . ?
O102 C102 Tc1 175.6(17) . . ?
O103 C103 Tc1 177.6(19) . . ?
O104 C104 Tc2 178.0(19) . . ?
O105 C105 Tc2 176.4(18) . . ?
O106 C106 Tc2 178.1(21) . . ?
O42 S41 O41 111.9(9) . . ?
O42 S41 O43 111.7(10) . . ?
O41 S41 O43 112.1(9) . . ?
O42 S41 C41 106.2(9) . . ?
O41 S41 C41 105.7(7) . . ?
O43 S41 C41 108.7(7) . . ?
C41 C42 C43 122.7(17) . . ?
C46 C41 C42 119.8(18) . . ?
C46 C41 S41 118.6(15) . . ?
C42 C41 S41 121.4(12) . . ?
C44 C43 C42 119.3(20) . . ?
C43 C44 C45 118.8(19) . . ?
C43 C44 C47 125.2(19) . . ?
C45 C44 C47 115.6(16) . . ?
C44 C45 C46 119.4(20) . . ?
C41 C46 C45 119.8(21) . . ?
O52 S51 O53 112.9 . . ?
O52 S51 O51 114.3 . . ?
O53 S51 O51 114.0 . . ?
O52 S51 C51 103.9 . . ?
O53 S51 C51 103.0 . . ?
O51 S51 C51 107.4 . . ?
C52 C51 C56 121.4(10) . . ?
C52 C51 S51 123.5 . . ?
C56 C51 S51 115.0(10) . . ?
C51 C52 C53 117.6(10) . . ?
C52 C53 C54 123.3(21) . . ?
C55 C54 C53 120.7(26) . . ?
C55 C54 C57 121.4(29) . . ?
C53 C54 C57 117.9(23) . . ?
C54 C55 C56 120.5(23) . . ?
C55 C56 C51 115.9(18) . . ?
C204 Tc4 C206 90.7(9) . . ?
C204 Tc4 C205 89.3(9) . . ?
C206 Tc4 C205 89.6(8) . . ?
C204 Tc4 S28 175.2(6) . . ?
C206 Tc4 S28 94.1(7) . . ?
C205 Tc4 S28 91.4(6) . . ?
C204 Tc4 S25 92.0(5) . . ?
C206 Tc4 S25 177.1(6) . . ?
C205 Tc4 S25 89.5(5) . . ?
S28 Tc4 S25 83.24(14) . . ?
C204 Tc4 S31 94.9(6) . . ?
C206 Tc4 S31 88.6(6) . . ?
C205 Tc4 S31 175.5(6) . . ?
S28 Tc4 S31 84.5(2) . . ?
S25 Tc4 S31 92.07(15) . . ?
C202 Tc3 C201 91.8(8) . . ?
C202 Tc3 C203 89.7(9) . . ?
C201 Tc3 C203 85.2(8) . . ?
C202 Tc3 S38 174.6(5) . . ?
C201 Tc3 S38 92.9(6) . . ?
C203 Tc3 S38 93.3(6) . . ?
C202 Tc3 S21 93.3(7) . . ?
C201 Tc3 S21 91.6(5) . . ?
C203 Tc3 S21 175.7(6) . . ?
S38 Tc3 S21 83.96(14) . . ?
C202 Tc3 S35 90.5(5) . . ?
C201 Tc3 S35 175.5(5) . . ?
C203 Tc3 S35 91.0(6) . . ?
S38 Tc3 S35 84.89(15) . . ?
S21 Tc3 S35 92.05(14) . . ?
C24 S25 C26 104.6(9) . . ?
C24 S25 Tc4 106.3(5) . . ?
C26 S25 Tc4 100.3(7) . . ?
C40 S21 C22 101.7(8) . . ?
C40 S21 Tc3 104.2(6) . . ?
C22 S21 Tc3 110.3(5) . . ?
C39 S38 C37 101.8(10) . . ?
C39 S38 Tc3 102.7(6) . . ?
C37 S38 Tc3 104.0(6) . . ?
C36 S35 C34 100.5(9) . . ?
C36 S35 Tc3 100.1(6) . . ?
C34 S35 Tc3 114.9(6) . . ?
C32 S31 C30 97.2(14) . . ?
C32 S31 Tc4 115.4(6) . . ?
C30 S31 Tc4 104.8(8) . . ?
C29 S28 C27 105.7(25) . . ?
C29 S28 Tc4 105.6(10) . . ?
C27 S28 Tc4 106.9(9) . . ?
C23 C24 S25 117.6(11) . . ?
O21 C23 C24 108.3(14) . . ?
O21 C23 C22 110.8(12) . . ?
C24 C23 C22 114.7(14) . . ?
C23 C22 S21 115.3(12) . . ?
C39 C40 S21 115.4(13) . . ?
C40 C39 S38 117.1(13) . . ?
C36 C37 S38 108.6(15) . . ?
C37 C36 S35 114.3(12) . . ?
C33 C34 S35 114.5(13) . . ?
C34 C33 C32 107.7(15) . . ?
C33 C32 S31 112.8(13) . . ?
C29 C30 S31 116.9(21) . . ?
C30 C29 S28 120.8(29) . . ?
C26 C27 S28 114.7(23) . . ?
C27 C26 S25 125.6(19) . . ?
O205 C205 Tc4 176.6(18) . . ?
O204 C204 Tc4 178.9(18) . . ?
O206 C206 Tc4 176.6(18) . . ?
O203 C203 Tc3 176.6(16) . . ?
O201 C201 Tc3 173.8(17) . . ?
O202 C202 Tc3 175.3(17) . . ?
O62 S61 O61 111.1(9) . . ?
O62 S61 O63 112.5(10) . . ?
O61 S61 O63 111.5(10) . . ?
O62 S61 C61 107.7(9) . . ?
O61 S61 C61 107.7(9) . . ?
O63 S61 C61 106.0(8) . . ?
C66 C61 C62 123.0(21) . . ?
C66 C61 S61 118.3(16) . . ?
C62 C61 S61 118.6(15) . . ?
C63 C62 C61 114.1(22) . . ?
C64 C63 C62 124.5(20) . . ?
C63 C64 C65 120.9(18) . . ?
C63 C64 C67 121.8(18) . . ?
C65 C64 C67 116.3(19) . . ?
C66 C65 C64 116.4(18) . . ?
C65 C66 C61 120.8(19) . . ?
O72 S71 O73 111.2(11) . . ?
O72 S71 O71 114.7(11) . . ?
O73 S71 O71 113.4(9) . . ?
O72 S71 C71 105.8(9) . . ?
O73 S71 C71 104.9(10) . . ?
O71 S71 C71 105.9(10) . . ?
C72 C71 C76 116.0(20) . . ?
C72 C71 S71 123.8(18) . . ?
C76 C71 S71 120.2(16) . . ?
C71 C72 C73 122.1(23) . . ?
C74 C73 C72 123.0(23) . . ?
C75 C74 C73 115.8(25) . . ?
C75 C74 C77 123.8(29) . . ?
C73 C74 C77 120.2(29) . . ?
C74 C75 C76 124.1(26) . . ?
C71 C76 C75 118.7(21) . . ?
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
Tc1 C101 1.90(2) . ?
Tc1 C103 1.94(2) . ?
Tc1 C102 1.97(2) . ?
Tc1 S18 2.460(4) . ?
Tc1 S15 2.478(4) . ?
Tc1 S1 2.482(4) . ?
Tc2 C106 1.86(2) . ?
Tc2 C104 1.89(2) . ?
Tc2 C105 1.89(3) . ?
Tc2 S8 2.446(5) . ?
Tc2 S5 2.453(5) . ?
Tc2 S11 2.482(5) . ?
S1 C2 1.79(2) . ?
S1 C20 1.81(2) . ?
S5 C6 1.80(2) . ?
S5 C4 1.85(2) . ?
S8 C7 1.76(2) . ?
S8 C9 1.83(2) . ?
S11 C10 1.76(2) . ?
S11 C12 1.81(2) . ?
S15 C16 1.77(2) . ?
S15 C14 1.82(2) . ?
S18 C19 1.81(2) . ?
S18 C17 1.81(2) . ?
C2 C3 1.54(2) . ?
C3 O1 1.41(2) . ?
C3 C4 1.52(3) . ?
C6 C7 1.63(3) . ?
C9 C10 1.60(3) . ?
C12 C13 1.54(2) . ?
C13 C14 1.47(2) . ?
C16 C17 1.50(2) . ?
C19 C20 1.55(2) . ?
C101 O101 1.13(2) . ?
C102 O102 1.14(2) . ?
C103 O103 1.14(2) . ?
C104 O104 1.18(2) . ?
C105 O105 1.24(3) . ?
C106 O106 1.18(2) . ?
S41 O42 1.397(13) . ?
S41 O41 1.420(12) . ?
S41 O43 1.443(12) . ?
S41 C41 1.76(2) . ?
C42 C41 1.37(2) . ?
C42 C43 1.39(3) . ?
C41 C46 1.33(2) . ?
C43 C44 1.37(3) . ?
C44 C45 1.41(3) . ?
C44 C47 1.56(2) . ?
C45 C46 1.44(3) . ?
S51 O52 1.46 . ?
S51 O53 1.46 . ?
S51 O51 1.46 . ?
S51 C51 1.76 . ?
C51 C52 1.37 . ?
C51 C56 1.47(2) . ?
C52 C53 1.38(2) . ?
C53 C54 1.39(4) . ?
C54 C55 1.33(3) . ?
C54 C57 1.54(3) . ?
C55 C56 1.45(3) . ?
Tc4 C204 1.87(2) . ?
Tc4 C206 1.93(2) . ?
Tc4 C205 1.95(2) . ?
Tc4 S28 2.455(5) . ?
Tc4 S25 2.466(4) . ?
Tc4 S31 2.484(4) . ?
Tc3 C202 1.91(2) . ?
Tc3 C201 1.92(2) . ?
Tc3 C203 1.93(2) . ?
Tc3 S38 2.455(4) . ?
Tc3 S21 2.463(4) . ?
Tc3 S35 2.475(5) . ?
S25 C24 1.81(2) . ?
S25 C26 1.81(2) . ?
S21 C40 1.77(2) . ?
S21 C22 1.77(2) . ?
S38 C39 1.71(2) . ?
S38 C37 1.88(2) . ?
S35 C36 1.80(2) . ?
S35 C34 1.83(2) . ?
S31 C32 1.79(2) . ?
S31 C30 1.84(3) . ?
S28 C29 1.72(3) . ?
S28 C27 1.82(3) . ?
C24 C23 1.50(2) . ?
C23 O21 1.45(2) . ?
C23 C22 1.53(2) . ?
C40 C39 1.50(2) . ?
C37 C36 1.50(3) . ?
C34 C33 1.50(2) . ?
C33 C32 1.52(2) . ?
C30 C29 1.49(4) . ?
C27 C26 1.31(3) . ?
O205 C205 1.13(2) . ?
O204 C204 1.18(2) . ?
O206 C206 1.15(2) . ?
O203 C203 1.14(2) . ?
O201 C201 1.16(2) . ?
O202 C202 1.17(2) . ?
S61 O62 1.431(14) . ?
S61 O61 1.439(14) . ?
S61 O63 1.449(15) . ?
S61 C61 1.77(2) . ?
C61 C66 1.39(2) . ?
C61 C62 1.40(3) . ?
C62 C63 1.40(3) . ?
C63 C64 1.34(3) . ?
C64 C65 1.43(3) . ?
C64 C67 1.58(3) . ?
C65 C66 1.39(3) . ?
S71 O72 1.378(14) . ?
S71 O73 1.453(14) . ?
S71 O71 1.47(2) . ?
S71 C71 1.73(2) . ?
C71 C72 1.36(3) . ?
C71 C76 1.38(3) . ?
C72 C73 1.38(3) . ?
C73 C74 1.37(3) . ?
C74 C75 1.29(3) . ?
C74 C77 1.39(3) . ?
C75 C76 1.45(3) . ?
O200 C200 1.31(3) . ?
O300 C300 1.28(3) . ?
O400 C400 1.27(3) . ?
O500 C500 1.29(3) . ?
