Synthesis and Characterization of Novel Oxotechnetium (99Tc and 99mTc) and Oxorhenium Complexes from the 2,2'-Bipyridine (NN)/Thiol (S) Mixed-Ligand System
Maria Papachristou; Ioannis C. Pirmettis; Charalambos Tsoukalas; Dionyssia Papagiannopoulou; Catherine Raptopoulou; Aris Terzis; Chariklia I. Stassinopoulou; Efstratios Chiotellis; Maria Pelecanou; Minas Papadopoulos; Inorganic Chemistry 42 (2003) 5778–5784; doi:10.1021/ic034368j

data_4314181
_publ_section_title
;
 Synthesis and Characterization of Novel Oxotechnetium (99Tc and 99mTc)
 and Oxorhenium Complexes from the 2,2'-Bipyridine (NN)/Thiol (S)
 Mixed-Ligand System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5778
_journal_page_last               5784
_journal_paper_doi               10.1021/ic034368j
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C31 H29 N2 O S3 Tc'
_chemical_formula_weight         639.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.81(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.12(1)
_cell_length_b                   14.394(6)
_cell_length_c                   8.801(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.3
_cell_volume                     2919(2)
_computing_cell_refinement
'Program LEAST (UCLA Cryst.package, C.E.Strouse 1994)'
_computing_data_collection
'Program COLLECT (UCLA Cryst.package, C.E.Strouse 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Cryst.package, C.E.Strouse 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       'theta-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  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5209
_diffrn_reflns_theta_max         24.51
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.735
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      1.44
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         4863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_obs          0.0376
_refine_ls_shift/esd_max         0.076
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.6542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1039
_refine_ls_wR_factor_obs         0.0921
_reflns_number_observed          3654
_reflns_number_total             4863
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic034368jsi20030724_032409_1.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.6542P] 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^)+(0.0415P)^2^+0.6542P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2918(2)
_cod_database_code               4314181