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_4322896
_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         '[Tc(CO)3(9S3)]Br'
_chemical_formula_sum            'C9 H12 Br O3 S3 Tc'
_chemical_formula_weight         442.28
_chemical_name_systematic
; 
[tricarbonyl(1,4,7-trithiacyclononane)technetium(I)]bromide 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.88(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.788(18)
_cell_length_b                   11.691(2)
_cell_length_c                   16.937(23)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      13.619
_cell_measurement_theta_min      8.943
_cell_volume                     2918(5)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        'CAD4 SDP'
_computing_molecular_graphics
'SCHAKAL (Keller 1989), 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      203(2)
_diffrn_measurement_device       'CAD 4'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K alpha'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8048
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        4.5
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         25
_exptl_absorpt_coefficient_mu    4.147
_exptl_absorpt_correction_T_max  0.9993
_exptl_absorpt_correction_T_min  0.9034
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_description       needle
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.155
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         7124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_restrained_S_obs      1.096
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_obs          0.0483
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+4.5946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0991
_refine_ls_wR_factor_obs         0.0779
_reflns_number_observed          4990
_reflns_number_total             7128
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980112f_1.cif
_cod_data_source_block           '[Tc(9-ane-S3)(CO)3]Br'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+4.5946P] 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^)+(0.0299P)^2^+4.5946P] 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        2917.6(53)
_cod_database_code               4322896