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
Roger Schibli; Roger Alberto; Ulrich Abram; Sonja Abram; André Egli; P. August Schubiger; Thomas A. Kaden; Inorganic Chemistry 37 (1998) 3509–3516; doi:10.1021/ic980112f

data_4322898
_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+0.001xFc^2^l^3^/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/[s^2^(Fo^2^)+( 0.1362P)^2^+1.1401P] where P=(Fo^2^+2Fc^2^)/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