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_4319132
_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 O2 P S3 Tc'
_chemical_formula_weight         511.55
_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-97
_cell_angle_alpha                73.0120(10)
_cell_angle_beta                 81.8690(10)
_cell_angle_gamma                79.7550(10)
_cell_formula_units_Z            2
_cell_length_a                   7.6294(4)
_cell_length_b                   12.2524(6)
_cell_length_c                   12.8379(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1124.29(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4878
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.403
_exptl_absorpt_correction_T_min  0.300
_exptl_absorpt_correction_type   'semiempirical using psi scans'
_exptl_crystal_colour            violett
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.8161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                3123
_reflns_number_total             3202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000828m_1.cif
_cod_data_source_block           Tc4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.8161P] 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^)+(0.0472P)^2^+0.8161P] 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               4319132