Synthesis and Characterization of Novel 99gTc(V) and Re(V) Complexes with Water-Soluble Tetraaza Diamido Dipyridino Ligands: Single-Crystal X-ray Structural Investigations of Mono- and Dinuclear Complexes
Laszlo Kurti; Dioni Papagiannopoulou; Minas Papadopoulos; Ioannis Pirmettis; Catherine P. Raptopoulou; Aris Terzis; Efstratios Chiotellis; Michael Harmata; Robert R. Kuntz; Raghoottama S. Pandurangi; Inorganic Chemistry 42 (2003) 2960–2967; doi:10.1021/ic020434q

data_4313522
_publ_section_title
;
 Synthesis and Characterization of Novel 99gTc(V) and Re(V) Complexes with
 Water-Soluble Tetraaza Diamido Dipyridino Ligands: Single-Crystal X-ray
 Structural Investigations of Mono- and Dinuclear Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2960
_journal_page_last               2967
_journal_paper_doi               10.1021/ic020434q
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C31 H38 N8 O11 Re2'
_chemical_formula_weight         1071.83
_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                78.725(7)
_cell_angle_beta                 76.133(7)
_cell_angle_gamma                67.656(8)
_cell_formula_units_Z            2
_cell_length_a                   11.646(3)
_cell_length_b                   11.850(3)
_cell_length_c                   14.396(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.3
_cell_volume                     1771.9(7)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_reduction
'Program REDEUCE (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Crystal Logixc Dual Goniometer diffractometer'
_diffrn_measurement_method       'thetah-2theta scans'
_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  0.0120
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6543
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        -0.2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.896
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            light-purple
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped'
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.234
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.5149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                5425
_reflns_number_total             6216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020434q_1.cif
_cod_data_source_block           she98
_cod_original_cell_volume        1771.8(7)
_cod_database_code               4313522