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_4319133
_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            'C19 H26 O P S4 Tc'
_chemical_formula_weight         527.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                95.4960(10)
_cell_angle_beta                 99.3760(10)
_cell_angle_gamma                92.2350(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3869(4)
_cell_length_b                   11.1578(6)
_cell_length_c                   12.3806(6)
_cell_measurement_temperature    293(2)
_cell_volume                     1136.08(10)
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5101
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_T_max  0.3628
_exptl_absorpt_correction_T_min  0.2254
_exptl_absorpt_correction_type   'semiempirical using psi scans'
_exptl_crystal_colour            light_violet
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       plate
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0098(10)
_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   0.748
_refine_ls_goodness_of_fit_obs   0.746
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.748
_refine_ls_restrained_S_obs      0.746
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_obs          0.0280
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+2.4851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0885
_refine_ls_wR_factor_obs         0.0855
_reflns_number_observed          3044
_reflns_number_total             3236
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000828m_2.cif
_cod_data_source_block           Tc5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0752P)^2^+2.4851P] 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^)+(0.0752P)^2^+2.4851P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319133