A Novel Seven-coordinate Technetium(IV) Complex: Synthesis and Characterization of [TcO(tpen)]2+ (tpen \δb N,N,N',N'-Tetrakis(2-pyridylmethyl)ethylenediamine)
Takashi Yoshimura; Masanori Kawai; Tsutomu Takayama; Tsutomu Sekine; Hiroshi Kudo; Atsushi Shinohara; Chemistry Letters 34 (2005) 1624–; doi:10.1246/cl.2005.1624

data_8000073
_publ_contact_author
;
 Takashi Yoshimura
 Department of Chemistry, Graduate School of Science, Osaka University,
 Toyonaka, Osaka, 560-0043, Japan
;
_publ_section_title
;
 A Novel Seven-coordinate Technetium(IV) Complex: Synthesis and
 Characterization of [TcO(tpen)]2+ (tpen \\db
 N,N,N',N'-Tetrakis(2-pyridylmethyl)ethylenediamine)
;
_journal_issue                   12
_journal_name_full               'Chemistry Letters'
_journal_page_first              1624
_journal_paper_doi               10.1246/cl.2005.1624
_journal_volume                  34
_journal_year                    2005
_chemical_formula_moiety         'C32 H40 Cl2 N6 O11 Tc'
_chemical_formula_sum            'C32 H40 Cl2 N6 O11 Tc'
_chemical_formula_weight         852.61
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      41
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_cell_angle_alpha                89
_cell_angle_beta                 90
_cell_angle_gamma                89
_cell_formula_units_Z            4
_cell_length_a                   12.546(1)
_cell_length_b                   25.351(4)
_cell_length_c                   11.584(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.7
_cell_measurement_theta_min      12.5
_cell_volume                     3684.3(9)
_computing_cell_refinement       WinAFC
_computing_data_collection       WinAFC
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.010
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2775
_diffrn_reflns_theta_max         27.50
_diffrn_standards_decay_%        0.09
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1756.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.48
_refine_ls_abs_structure_Flack   0.60(8)
_refine_ls_extinction_coef       0.0000
_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_ref   1.063
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2348
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                1723
_reflns_number_total             2348
_reflns_threshold_expression     >2.0sigma(I)
_cod_original_sg_symbol_H-M      'A b a 2      '
_cod_original_formula_sum        'C32 H40 Cl2 N6 O11 Tc '
_cod_database_code               8000073