Synthesis and Characterization of Novel Trigonal Bipyramidal Technetium(III) Mixed-Ligand Complexes with SES/S/P Coordination (E = O, N(CH3), S)
Hans-Jürgen Pietzsch; Francesco Tisato; Fiorenzo Refosco; Peter Leibnitz; Antje Drews; Sepp Seifert; Hartmut Spies; Inorganic Chemistry 40 (2001) 59–64; doi:10.1021/ic000828m

data_4319134
_publ_section_title
;
 Synthesis and Characterization of Novel Trigonal Bipyramidal
 Technetium(III) Mixed-Ligand Complexes with SES/S/P Coordination (E = O,
 N(CH3), S)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              59
_journal_page_last               64
_journal_paper_doi               10.1021/ic000828m
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C20 H29 N O P S3 Tc'
_chemical_formula_weight         524.59
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.7080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3054(5)
_cell_length_b                   9.4678(4)
_cell_length_c                   18.7909(7)
_cell_measurement_temperature    293(2)
_cell_volume                     2325.92(16)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9673
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.299
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   SEMIEMPIRICAL
_exptl_crystal_colour            dark_violet
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.064
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_obs          0.0238
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+1.1389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0665
_refine_ls_wR_factor_obs         0.0594
_reflns_number_observed          3171
_reflns_number_total             3344
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000828m_3.cif
_cod_data_source_block           Tc6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+1.1389P] 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^)+(0.0290P)^2^+1.1389P] 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        2325.9(2)
_cod_database_code               4319134