Two mononuclear Tc complexes: [2,2'-(3-phenylpropylimino)- and [2,2'-(propylimino)bis(ethanethiolato)](4-methoxybenzenethiolato)oxidotechnate(V)
Franziska Emmerling; Werner Kraus; Bernhard Noll; Steffi Noll; Hans-Jürgen Pietzsch; Acta Crystallographica Section C 63 (2007) m579–m582; doi:10.1107/S0108270107052870

data_2016302
_publ_section_title
;Two mononuclear Tc complexes: [2,2'-(3-phenylpropylimino)- and
 [2,2'-(propylimino)bis(ethanethiolato)](4-methoxybenzenethiolato)oxidotechnate(V)
;
_journal_coeditor_code           BG3060
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m579
_journal_page_last               m582
_journal_paper_doi               10.1107/S0108270107052870
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Tc (C14 H21 N S2) (C7 H7 O S) O]'
_chemical_formula_moiety         'C21 H28 N O2 S3 Tc'
_chemical_formula_sum            'C21 H28 N O2 S3 Tc'
_chemical_formula_weight         520.62
_chemical_name_systematic
;
(4-methoxybenzenethiolato-\kS)oxido[2,2'-(3-
phenylpropylimino)bis(ethanethiolato)-\k^3^S,N,S']technetium(V)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.913(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.885(7)
_cell_length_b                   7.247(4)
_cell_length_c                   14.885(7)
_cell_measurement_reflns_used    775
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.632
_cell_measurement_theta_min      3.0645
_cell_volume                     1152.9(11)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6818
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.91
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.566
_refine_diff_density_min         -0.809
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4523
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0606P)^2^+3.45P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1435
_reflns_number_gt                3581
_reflns_number_total             4523
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg3060.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21
_cod_database_code               2016302
_cod_database_fobs_code          2016302