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_4318754
_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(dppmO)2](PF6)'
_chemical_formula_sum            'C50 H44 Cl2 F6 O2 P5 Tc'
_chemical_formula_weight         1114.60
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 100.5630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   35.3200(11)
_cell_length_b                   11.5242(4)
_cell_length_c                   42.0610(12)
_cell_measurement_temperature    183(2)
_cell_volume                     16830.2(9)
_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      183(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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            27277
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       parallelpip
_exptl_crystal_F_000             6792
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00011(2)
_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   1.175
_refine_ls_goodness_of_fit_obs   1.221
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         9043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.192
_refine_ls_restrained_S_obs      1.221
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_obs          0.0810
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+196.5097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1960
_refine_ls_wR_factor_obs         0.1858
_reflns_number_observed          7827
_reflns_number_total             9045
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020032i_5.cif
_cod_data_source_block           99180
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0680P)^2^+196.5097P] 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^)+(0.0680P)^2^+196.5097P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4318754