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_4322897
_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(tosylat)2(18-Krone-S6)]'
_chemical_formula_sum            'C32 H38 O12 S8 Tc2'
_chemical_formula_weight         1067.10
_chemical_name_common            '[Tc2(CO)6(tosylat)2(18-Krone-S6)]'
_chemical_name_systematic
Hexacarbonyl(18-crown-S6-S1,S2,S4,S5)bis(4-toluenedisulfonato-O)ditechnetium(I)
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.84(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.073(4)
_cell_length_b                   9.288(1)
_cell_length_c                   17.898(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      14.69
_cell_volume                     4270.5(11)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        'CAD4, SDP'
_computing_molecular_graphics
'SCHAKAL (Keller, 1992), ZORTEP (Zsolnai, 1994)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3927
_diffrn_reflns_theta_max         64.93
_diffrn_reflns_theta_min         5.02
_diffrn_standards_decay_%        2.1
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.396
_exptl_absorpt_correction_T_max  0.9984
_exptl_absorpt_correction_T_min  0.7669
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         .582
_refine_diff_density_min         -.717
_refine_diff_density_rms         .103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.054
_refine_ls_hydrogen_treatment    refined
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.054
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_obs          0.0401
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0396P)^2^+15.7433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1028
_refine_ls_wR_factor_obs         0.0890
_reflns_number_observed          2654
_reflns_number_total             3585
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980112f_2.cif
_cod_data_source_block           '[Tc2(tosylate)2(18-ane-S6)(CO)6]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0396P)^2^+15.7433P] 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^)+( 0.0396P)^2^+15.7433P]
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        4270(1)
_cod_database_code               4322897