Reduction of the Pertechnetate Anion with Bidentate Phosphine Ligands
Evan Freiberg; William M. Davis; Terrence Nicholson; Alan Davison; Alun G. Jones; Inorganic Chemistry 41 (2002) 5667–5674; doi:10.1021/ic020032i

data_4318751
_publ_section_title
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 Reduction of the Pertechnetate Anion with Bidentate Phosphine Ligands
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5667
_journal_page_last               5674
_journal_paper_doi               10.1021/ic020032i
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '[TcCl2(dppm)2](PF6)'
_chemical_formula_sum            'C53 H50 Cl2 F6 O P5 Tc'
_chemical_formula_weight         1140.68
_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                87.726(2)
_cell_angle_beta                 80.318(2)
_cell_angle_gamma                72.725(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1601(13)
_cell_length_b                   12.9798(14)
_cell_length_c                   17.2293(18)
_cell_measurement_temperature    183(2)
_cell_volume                     2559.6(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10476
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            garnet
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          .22
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .38
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0007(3)
_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   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         7284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+2.9359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                6601
_reflns_number_total             7284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020032i_2.cif
_cod_data_source_block           00210t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4318751