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_4318750
_publ_section_title
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 Reduction of the Pertechnetate Anion with Bidentate Phosphine Ligands
;
_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
_chemical_formula_sum            'C50 H44 Cl2 P4 Tc'
_chemical_formula_weight         937.63
_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
_cell_angle_alpha                92.771(2)
_cell_angle_beta                 104.474(2)
_cell_angle_gamma                104.771(2)
_cell_formula_units_Z            1
_cell_length_a                   11.0256(11)
_cell_length_b                   11.2695(11)
_cell_length_c                   11.7812(12)
_cell_measurement_temperature    185(2)
_cell_volume                     1360.7(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      185(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4126
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.8887
_exptl_absorpt_correction_T_min  0.7920
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       block
_exptl_crystal_F_000             481
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0011(17)
_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_all   1.182
_refine_ls_goodness_of_fit_obs   1.214
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         2533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.231
_refine_ls_restrained_S_obs      1.214
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_obs          0.0755
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+11.0815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1901
_refine_ls_wR_factor_obs         0.1767
_reflns_number_observed          2265
_reflns_number_total             2535
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020032i_1.cif
_cod_data_source_block           99113
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+11.0815P] 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^)+(0.0634P)^2^+11.0815P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4318750